首页 期刊 论文 学科刊群 资讯 加盟 关于
EN
image
Article(id=1322947109468635335, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945651499213732, articleNumber=null, orderNo=null, doi=10.3724/SP.J.1123.2024.11028, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1734105600000, receivedDateStr=2024-12-14, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793344770065, onlineDateStr=2026-10-30, pubDate=1751904000000, pubDateStr=2025-07-08, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793344770065, onlineIssueDateStr=2026-10-30, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793344770065, creator=13701087609, updateTime=1793344770065, updator=13701087609, issue=Issue{id=1322945651499213732, tenantId=1146029695717560320, journalId=1283840372199657495, year='2025', volume='43', issue='7', pageStart='713', pageEnd='835', issueExtLink='null', onlineDate='null', pubDate='1751904000000', pubDateStr='2025-07-08', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793344422459, creator='13701087609', updateTime=1793345275766, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322949230586889175, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945651499213732, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322949230586889176, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945651499213732, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=756, endPage=766, ext={EN=ArticleExt(id=1322947109934203080, articleId=1322947109468635335, tenantId=1146029695717560320, journalId=1283840372199657495, language=EN, title=Fast determination of per- and polyfluoroalkyl substances in human serum by cold-induced phase separation coupled with liquid chromatography-tandem mass spectrometry, columnId=1284557502633185292, journalTitle=Chinese Journal of Chromatography, columnName=Articles, runingTitle=null, highlight=null, articleAbstract=

Per- and polyfluoroalkyl substances （PFASs） are a large group of synthetic chemicals that have been widely used in various industrial and commercial products owing to their unique physicochemical properties. However， accumulating evidence suggests that PFASs are persistent， transmissive over long distances， bioaccumulative， and toxic； consequently， their adverse effects on ecosystems and humans is of widespread concern. Serum is the most commonly used human matrix for assessing internal exposure to environmental pollutants， and several analytical methods have been developed to measure PFASs in sera. Current methods are generally fast， convenient， and robust； however， their pretreatment steps require large amounts of organic solvents and materials， such as solid-phase extraction cartridges and/or sorbents. In this study， a novel and low-cost analytical method based on cold-induced phase separation （CIPS） strategy was developed for the simultaneous determination of 31 legacy and emerging PFASs in serum. The core mechanism and distinctive feature of CIPS involves cooling an acetonitrile-water （ACN-water） mixture at a low temperature to produce two clear-cut layers： one with a high ACN proportion （the ACN layer） and an aqueous layer （water layer）. Certain chemicals are significantly enriched in the ACN layer during cooling； at the same time， impurities， especially water-soluble impurities， remain in the aqueous layer. CIPS only requires the temperature to be varied， and no external impurities are introduced during pretreatment， which dramatically reduces material costs and avoids new impurities from intervening. Our method involves the following procedure： serum was drawn accurately （0.2 mL） into a 1.5 mL Eppendorf （EP） tube， 2 ng of each isotopically labeled internal standard was added， the mixture is vortexed， and 350 µL of ACN was added， followed by vortexing and ultrasonic extraction. Subsequently， 450 µL of water is added to adjust the volume proportion of ACN to 35% （the volume percentage of ACN in the total solution）. The protein at the bottom of the tube was collected following centrifugation at 15 000 r/min for 10 min， and the supernatant was transferred to a 1 mL syringe. The syringe was frozen in a -20 ℃ refrigerator for 1 h to obtain the two layers， after which the upper layer （approximately 80–100 μL） containing ACN and the target compounds was finally transferred to a glass vial for instrumental analysis. Liquid chromatography coupled with triple quadrupole mass spectrometry augmented with electrospray ionization （LC-ESI-MS/MS） was used to quantify the PFASs. The analytes were separated using a C18 column， with methanol and 2 mmol/L of ammonium formate-H2O used as mobile phases. Linearities， limits of detection （LODs） and， limits of quantification （LOQs）， recoveries， precisions， and matrix effects were determined under the optimal conditions. The LODs and LOQs of PFASs in serum were 0.01–25 and 0.03–83 pg/mL， respectively. Under two spiked levels， namely 5 ng/mL and 25 ng/mL， average recoveries ranged between 60.5% and 129.6%， with relative standard deviations （RSDs） of less than 22.8%. Under 5 pg/mL as LOD spiked level， average recoveries ranged between 61.6% and 199.1%，with RSDs<29.4%. While matrix-effect testing revealed slightly enhanced signals， the use of isotopically labeled internal standards compensated for these effects. Real samples were subsequently analyzed， with 50 human serum samples collected in first trimester of pregnancy women living in the Shunyi District， Beijing. Nine PFASs exhibited high detection frequencies （>80%）， which suggests that PFASs are ubiquitous in the population. The median and mean levels of Σ31PFASs （sum of 31 PFASs） in serum were 21.8 and 22.9 ng/mL， respectively， and the range was 0.456-73.9 ng/mL. Both legacy and emerging PFASs were detected at high frequencies and contamination levels， which suggests that they are widely used. In summary， the method developed in this study is fast， sensitive， and solvent- and material-efficient； it is also very linear and highly accurate， and exhibits satisfactory extraction recovery and enrichment factors； hence， it is suitable for surveying large populations as well as for use in environmental epidemiology.

, authors=Jiandi WANG1, 2, Yiwei WANG1, Jiaxin WU1, Zhixiong SHI1, *, authorsList=Jiandi WANG, Yiwei WANG, Jiaxin WU, Zhixiong SHI, authorCompany=null, correspAuthors=Zhixiong SHI, authorNote=null, correspAuthorsNote=null, copyrightStatement=This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1322947112467562702, articleId=1322947109468635335, tenantId=1146029695717560320, journalId=1283840372199657495, language=CN, title=冷冻诱导相分离结合液相色谱-串联质谱快速测定人血清中全氟和多氟烷基化合物, columnId=1284557502792568846, journalTitle=色谱, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

全氟和多氟烷基化合物（per- and polyfluoroalkyl substances， PFASs）的广泛应用带来了显著的环境污染与人群健康风险。血清测定是开展PFASs的人群内暴露评估及人群流行病学研究的基础，因此亟需建立可快速准确测定大规模人群血清中PFASs 的分析技术。本研究建立了可快速测定血清中31种PFASs的方法。血清中加入稳定性同位素内标后采用乙腈萃取，通过集净化与富集为一体的冷冻诱导相分离处理后，采用液相色谱-电喷雾电离-串联质谱在选择反应监测模式下采集质谱数据，内标法定量。对仪器分析参数和冷冻诱导相分离条件进行了优化。确定以乙腈为萃取溶剂，冷冻诱导相分离时溶液中乙腈体积分数为35%，-20 ℃下冷冻1 h为最佳样品前处理条件。在优化后的条件下，PFASs在0.5~20 ng/mL范围内线性良好，检出限为0.01~25 pg/mL，定量限为0.03~83 pg/mL；在5和25 ng/mL加标水平下，PFASs的平均回收率为60.5%~129.6%，相对标准偏差≤22.8%；在5 pg/mL定量限加标水平下，PFASs的平均回收率为61.6%~199.1%，RSD≤29.4%。采用所建立的方法测定了北京市顺义区50份孕妇血清样本，其中PFASs总和含量中值与均值分别为21.8和22.9 ng/mL，含量范围为0.456~73.9 ng/mL。有24种PFASs检出率在30%以上，其中9种检出率大于80%。高检出率表明PFASs的人群暴露普遍存在，同时胎儿可通过母-婴传递暴露于PFASs。此外传统PFASs和新型替代品检出率和污染水平均较高，人群暴露和潜在健康风险不容忽视。本研究所建立的方法操作简单，有机溶剂和耗材消耗极少，灵敏度和稳定性良好，适用于大规模人群监测与环境流行病学研究。

, authors=王建迪1, 2, 王仪伟1, 吴佳欣1, 施致雄1, *, authorsList=王建迪, 王仪伟, 吴佳欣, 施致雄, authorCompany=null, correspAuthors=施致雄, authorNote=null, correspAuthorsNote=
*E-mail：.
, copyrightStatement=Copyright © 2025 Editorial office of Chinese Journal of Chromatography
本文是开放获取文章，遵循CC BY 4.0协议
, copyrightOwner=Editorial office of Chinese Journal of Chromatography, extLink=null, articleAbsUrl=null, sourceXml=FdGx9OHLNif7SaazXcFjaQ==, magXml=r9dC6B22zOIgfP+MUGb7CQ==, pdfUrl=null, pdf=lNNSkKGgp2vwdtb8HHOYgg==, pdfFileSize=1896207, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=lr+NhoR8jk//qOH558WSiQ==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=lmh7KwpA3wThWie3gSQMgg==, mapNumber=null, fund=null)}, authors=[Author(id=1322947224870728140, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947224958808527, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947224870728140, language=EN, stringName=Jiandi WANG, firstName=Jiandi, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, address=1. School of Public Health，Capital Medical University，Beijing 100069，China
2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225172718032, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947224870728140, language=CN, stringName=王建迪, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, address=1.首都医科大学公共卫生学院，北京 100069
2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)]), AuthorCompany(id=1322947224765870536, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224782647753, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China), AuthorCompanyExt(id=1322947224795230666, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300)])]), Author(id=1322947225353073106, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=1, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947225428570580, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225353073106, language=EN, stringName=Yiwei WANG, firstName=Yiwei, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225491485141, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225353073106, language=CN, stringName=王仪伟, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])]), Author(id=1322947225554399703, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=2, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947225663451609, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225554399703, language=EN, stringName=Jiaxin WU, firstName=Jiaxin, middleName=null, lastName=WU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225810252250, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225554399703, language=CN, stringName=吴佳欣, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])]), Author(id=1322947225927692764, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=3, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=szx0127@ccmu.edu.cn, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1322947226179351007, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225927692764, language=EN, stringName=Zhixiong SHI, firstName=Zhixiong, middleName=null, lastName=SHI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947226485535200, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225927692764, language=CN, stringName=施致雄, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])])], keywords=[Keyword(id=1322947226993045985, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, orderNo=1, keyword=per- and polyfluoroalkyl substances （PFASs）), Keyword(id=1322947227060154850, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, orderNo=2, keyword=cold-induced), Keyword(id=1322947227278258659, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, orderNo=3, keyword=serum), Keyword(id=1322947227404087780, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, orderNo=4, keyword=isotope dilution), Keyword(id=1322947229073420773, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, orderNo=5, keyword=liquid chromatography-tandem mass spectrometry （LC-MS/MS）), Keyword(id=1322947229136335334, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, orderNo=1, keyword=全氟和多氟烷基化合物), Keyword(id=1322947229211832807, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, orderNo=2, keyword=冷冻诱导), Keyword(id=1322947229270553064, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, orderNo=3, keyword=血清), Keyword(id=1322947229341856233, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, orderNo=4, keyword=同位素稀释), Keyword(id=1322947229442519530, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, orderNo=5, keyword=液相色谱-串联质谱)], refs=[Reference(id=1322947231610974717, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=36, issue=11, pageStart=1607, pageEnd=null, url=null, language=null, rfNumber=1, rfOrder=0, authorNames=Wang Y W, Zhang Q R, Yu N Y, journalName=Progress in Chemistry, refType=null, unstructuredReference=Wang Y W， Zhang Q R， Yu N Y， et al. Progress in Chemistry， 2024， 36（11）： 1607, articleTitle=null, refAbstract=null), Reference(id=1322947231682277886, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=36, issue=11, pageStart=1607, pageEnd=null, url=null, language=null, rfNumber=1, rfOrder=1, authorNames=王亚韡, 张秋瑞, 于南洋, journalName=化学进展, refType=null, unstructuredReference=王亚韡， 张秋瑞， 于南洋， 等. 化学进展， 2024， 36（11）： 1607, articleTitle=null, refAbstract=null), Reference(id=1322947231745192447, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=472, issue=null, pageStart=134556, pageEnd=null, url=null, language=null, rfNumber=2, rfOrder=2, authorNames=Xing W Y, Sun J N, Liu F H, journalName=J Hazard Mater, refType=null, unstructuredReference=Xing W Y， Sun J N， Liu F H， et al. J Hazard Mater， 2024， 472： 134556, articleTitle=null, refAbstract=null), Reference(id=1322947231808107008, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=332, issue=10, pageStart=785, pageEnd=null, url=null, language=null, rfNumber=3, rfOrder=3, authorNames=Criswell R, Fleisch A F, Ducatman A, journalName=JAMA, refType=null, unstructuredReference=Criswell R， Fleisch A F， Ducatman A. JAMA， 2024， 332（10）： 785, articleTitle=null, refAbstract=null), Reference(id=1322947231887798785, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=2, pageStart=217, pageEnd=null, url=null, language=null, rfNumber=4, rfOrder=4, authorNames=Zhang M Y, Cao Y, Li X, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=Zhang M Y， Cao Y， Li X， et al. Chinese Journal of Chromatography， 2024， 42（2）： 217, articleTitle=null, refAbstract=null), Reference(id=1322947233552937474, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=2, pageStart=217, pageEnd=null, url=null, language=null, rfNumber=4, rfOrder=5, authorNames=张明烨, 曹衍, 李想, journalName=色谱, refType=null, unstructuredReference=张明烨， 曹衍， 李想， 等. 色谱， 2024， 42（2）： 217, articleTitle=null, refAbstract=null), Reference(id=1322947233653600771, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=8, pageStart=731, pageEnd=null, url=null, language=null, rfNumber=5, rfOrder=6, authorNames=Feng H, Zhang W, He B S, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=Feng H， Zhang W， He B S， et al. Chinese Journal of Chromatography， 2024， 42（8）： 731, articleTitle=null, refAbstract=null), Reference(id=1322947233771041284, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=8, pageStart=731, pageEnd=null, url=null, language=null, rfNumber=5, rfOrder=7, authorNames=冯灏, 张炜, 何保山, journalName=色谱, refType=null, unstructuredReference=冯灏， 张炜， 何保山， 等. 色谱， 2024， 42（8）： 731, articleTitle=null, refAbstract=null), Reference(id=1322947233871704581, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=8, pageStart=740, pageEnd=null, url=null, language=null, rfNumber=6, rfOrder=8, authorNames=Liu X Q, Liu Z Z, Wang M Y, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=Liu X Q， Liu Z Z， Wang M Y， et al. Chinese Journal of Chromatography， 2024， 42（8）： 740, articleTitle=null, refAbstract=null), Reference(id=1322947233947202054, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=8, pageStart=740, pageEnd=null, url=null, language=null, rfNumber=6, rfOrder=9, authorNames=刘小琦, 刘真真, 王美玉, journalName=色谱, refType=null, unstructuredReference=刘小琦， 刘真真， 王美玉， 等. 色谱， 2024， 42（8）： 740, articleTitle=null, refAbstract=null), Reference(id=1322947234014310919, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=43, issue=3, pageStart=252, pageEnd=null, url=null, language=null, rfNumber=7, rfOrder=10, authorNames=Lin Q, Wang J, Li J J, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=Lin Q， Wang J， Li J J， et al. Chinese Journal of Chromatography， 2024， 43（3）： 252, articleTitle=null, refAbstract=null), Reference(id=1322947234077225480, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=43, issue=3, pageStart=252, pageEnd=null, url=null, language=null, rfNumber=7, rfOrder=11, authorNames=林强, 王健, 李晶晶, journalName=色谱, refType=null, unstructuredReference=林强， 王健， 李晶晶， 等. 色谱， 2024， 43（3）： 252, articleTitle=null, refAbstract=null), Reference(id=1322947234165305865, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=41, issue=4, pageStart=375, pageEnd=null, url=null, language=null, rfNumber=8, rfOrder=12, authorNames=Wang Z, Zhang B Y, Zhang J M, journalName=Journal of Environmental and Occupational Medicine, refType=null, unstructuredReference=Wang Z， Zhang B Y， Zhang J M， et al. Journal of Environmental and Occupational Medicine， 2024， 41（4）： 375, articleTitle=null, refAbstract=null), Reference(id=1322947234228220426, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=41, issue=4, pageStart=375, pageEnd=null, url=null, language=null, rfNumber=8, rfOrder=13, authorNames=王铮, 张博雅, 张济明, journalName=环境与职业医学, refType=null, unstructuredReference=王铮， 张博雅， 张济明， 等. 环境与职业医学， 2024， 41（4）： 375, articleTitle=null, refAbstract=null), Reference(id=1322947234307912203, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2025, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=9, rfOrder=14, authorNames=Xiao K T, Zhang B N, Wang Y C, journalName=Environmental Chemistry, refType=null, unstructuredReference=Xiao K T， Zhang B N， Wang Y C， et al. Environmental Chemistry， 2025. DOI： 10.7524/j.issn.0254-6108.2024022102, articleTitle=null, refAbstract=null), Reference(id=1322947234379215372, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2025, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=9, rfOrder=15, authorNames=肖锴婷, 张博钠, 王祎纯, journalName=环境化学, refType=null, unstructuredReference=肖锴婷， 张博钠， 王祎纯， 等. 环境化学， 2025. DOI： 10.7524/j.issn.0254-6108.2024022102, articleTitle=null, refAbstract=null), Reference(id=1322947234454712845, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2019, volume=9, issue=5, pageStart=494, pageEnd=null, url=null, language=null, rfNumber=10, rfOrder=16, authorNames=Xie L N, Zhang H J, Hou S S, journalName=Journal of Environmental Hygiene, refType=null, unstructuredReference=Xie L N， Zhang H J， Hou S S， et al. Journal of Environmental Hygiene， 2019， 9（5）： 494, articleTitle=null, refAbstract=null), Reference(id=1322947234584736270, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2019, volume=9, issue=5, pageStart=494, pageEnd=null, url=null, language=null, rfNumber=10, rfOrder=17, authorNames=谢琳娜, 张海婧, 侯沙沙, journalName=环境卫生学杂志, refType=null, unstructuredReference=谢琳娜， 张海婧， 侯沙沙， 等. 环境卫生学杂志， 2019， 9（5）： 494, articleTitle=null, refAbstract=null), Reference(id=1322947234651845135, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2022, volume=94, issue=10, pageStart=4227, pageEnd=null, url=null, language=null, rfNumber=11, rfOrder=18, authorNames=Liu Z, Chen D, Lyu B, journalName=Anal Chem, refType=null, unstructuredReference=Liu Z， Chen D， Lyu B， et al. Anal Chem， 2022， 94（10）： 4227, articleTitle=null, refAbstract=null), Reference(id=1322947234718954000, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2024, volume=416, issue=28, pageStart=6663, pageEnd=null, url=null, language=null, rfNumber=12, rfOrder=19, authorNames=Wu J, Yao S, Wang Y, journalName=Anal Bioanal Chem, refType=null, unstructuredReference=Wu J， Yao S， Wang Y， et al. Anal Bioanal Chem， 2024， 416（28）： 6663, articleTitle=null, refAbstract=null), Reference(id=1322947234781868561, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2020, volume=328, issue=null, pageStart=127113, pageEnd=null, url=null, language=null, rfNumber=13, rfOrder=20, authorNames=Li S, Ren J, Zhang Y, journalName=Food Chem, refType=null, unstructuredReference=Li S， Ren J， Zhang Y， et al. Food Chem， 2020， 328： 127113, articleTitle=null, refAbstract=null), Reference(id=1322947234874143250, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2017, volume=1506, issue=null, pageStart=128, pageEnd=null, url=null, language=null, rfNumber=14, rfOrder=21, authorNames=Shao G, Agar J, Giese R W, journalName=J Chromatog A, refType=null, unstructuredReference=Shao G， Agar J， Giese R W. J Chromatog A， 2017， 1506： 128, articleTitle=null, refAbstract=null), Reference(id=1322947234966417939, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2021, volume=1659, issue=null, pageStart=462589, pageEnd=null, url=null, language=null, rfNumber=15, rfOrder=22, authorNames=Qi P P, Wang J, Liu Z Z, journalName=J Chromatogr A, refType=null, unstructuredReference=Qi P P， Wang J， Liu Z Z， et al. J Chromatogr A， 2021， 1659： 462589, articleTitle=null, refAbstract=null), Reference(id=1322947235025138196, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2020, volume=41, issue=12, pageStart=120, pageEnd=null, url=null, language=null, rfNumber=16, rfOrder=23, authorNames=Guo C H, Fan Y S, Qiao Y Z, journalName=Progress in Veterinary Medicine, refType=null, unstructuredReference=Guo C H， Fan Y S， Qiao Y Z， et al. Progress in Veterinary Medicine， 2020， 41（12）： 120, articleTitle=null, refAbstract=null), Reference(id=1322947235125801493, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, doi=null, pmid=null, pmcid=null, year=2020, volume=41, issue=12, pageStart=120, pageEnd=null, url=null, language=null, rfNumber=16, rfOrder=24, authorNames=郭聪慧, 范玉珊, 乔延召, journalName=动物医学进展, refType=null, unstructuredReference=郭聪慧， 范玉珊， 乔延召， 等. 动物医学进展， 2020， 41（12）： 120, articleTitle=null, refAbstract=null)], funds=[Fund(id=1322947230793085429, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=null, language=EN, fundingSource=Capital’s Funds for Health Improvement and Research（CFH，2022-2G-4264）, fundOrder=null, country=null), Fund(id=1322947231023772150, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=null, language=CN, fundingSource=首都卫生发展科研专项（首发2022-2G-4264）, fundOrder=null, country=null), Fund(id=1322947231103463927, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=2024-2G-7103, language=EN, fundingSource=Capital’s Funds for Health Improvement and Research(2024-2G-7103), fundOrder=null, country=null), Fund(id=1322947231170572792, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=2024-2G-7103, language=CN, fundingSource=首都卫生发展科研专项(2024-2G-7103), fundOrder=null, country=null), Fund(id=1322947231246070265, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=KZ20231002549, language=EN, fundingSource=R&D Program of Beijing Municipal Education Commission(KZ20231002549), fundOrder=null, country=null), Fund(id=1322947231313179130, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=KZ20231002549, language=CN, fundingSource=北京市教育委员会科技计划重点项目(KZ20231002549), fundOrder=null, country=null), Fund(id=1322947231392870907, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=2023-03-46, language=EN, fundingSource=Talent Development Plan for High-level Public Health Technical Personnel Project in Beijing(2023-03-46), fundOrder=null, country=null), Fund(id=1322947231455785468, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, awardId=2023-03-46, language=CN, fundingSource=北京市高层次公共卫生技术人才建设项目(2023-03-46), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)]), AuthorCompany(id=1322947224765870536, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224782647753, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China), AuthorCompanyExt(id=1322947224795230666, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300)])], figs=[ArticleFig(id=1322947229824201195, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, label=Fig. 1, caption=Total ion chromatogram of the 31 PFASs （5 ng/mL） in the standard solution

Sequence number of each peak match to the ordinal in Table 1.

, figureFileSmall=s/TWZPdO2y0s/xMMGzna3Q==, figureFileBig=lr+NhoR8jk//qOH558WSiQ==, tableContent=null), ArticleFig(id=1322947229895504364, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, label=图1, caption=31种PFASs标准溶液（5 ng/mL）的总离子流色谱图, figureFileSmall=s/TWZPdO2y0s/xMMGzna3Q==, figureFileBig=lr+NhoR8jk//qOH558WSiQ==, tableContent=null), ArticleFig(id=1322947229979390445, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, label=Fig. 2, caption=（a） Enrichment factors and （b） extraction recoveries of PFASs under various acetonitrile proportions （n=5）, figureFileSmall=rdAgVyHMVNhaWECc1whW2Q==, figureFileBig=WbpD0OIdfRQN6ntRjuRYPA==, tableContent=null), ArticleFig(id=1322947230033916398, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, label=图2, caption=不同乙腈比例下PFASs的（a）富集系数和（b）萃取回收率（n=5）, figureFileSmall=rdAgVyHMVNhaWECc1whW2Q==, figureFileBig=WbpD0OIdfRQN6ntRjuRYPA==, tableContent=null), ArticleFig(id=1322947230092636655, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, label=Table 1, caption=

Retention times and MS parameters of the 31 per- and polyfluoroalkyl substances （PFASs） and 9 internal standards（Continued）

, figureFileSmall=null, figureFileBig=null, tableContent=
No.CompoundChinese nameRT/minPrecursor ion （m/z）Product ion （m/z）CE/eVRF/VIS
1perfluorobutyric acid （PFBA）全氟丁酸3.77213.1169.0*103013C4-PFBA
180.810
182.817
2perfluorobutanesulfonate （PFBS）全氟丁烷磺酸盐6.02298.980.0*3310318O2-PFHxS
99.030
218.923
3sodium 1H，1H，2H，2H-perfluorohexane sulfonate（4∶2） （4∶2FTS）1H，1H，2H，2H-全氟己烷磺酸钠6.65327.080.4287713C4-PFBA
286.925
306.9*20
4perfluorohexanoic acid （PFHxA）全氟己酸6.78312.9119.1213013C2-PFHxA
269.0*10
295.217
5perfluoropentanesulfonic acid （PFPeS）全氟膦酸6.9349.180.0*3510518O2-PFHxS
99.032
119.033
6hexafluoropropylene oxide dimer acid （HFPO-DA）六氟环氧丙烷二聚酸6.93285.0119.0296213C2-PFHxA
169.0*10
185.019
7perfluorobutane sulfonamide （FBSA）全氟丁烷磺酰胺6.99298.078.0*257013C4-PFOA
119.019
218.819
8perfluoroheptanoic acid （PHHpA）全氟庚酸7.46362.9169.0173218O2-PFHxS
281.117
319.0*10
9sodium dodecafluoro-3H-4，8-dioxanonanoate （NaDONA）十二氟-3H-4，8-二氧六烯酸钠7.48377.085.0293813C4-PFOA
251.0*10
358.910
10dodecafluoro-3H-4，8-dioxanonane sodium salt （DONA）十二氟-3H-4，8-二氧杂壬酸钠7.53376.7250.9*104013C4-PFOA
11perfluorohexanesulfonate （PFHxS）全氟己烷磺酸7.53399.180.0*2311218O2-PFHxS
99.037
319.035
12perfluorohexyl ethyl vinyl ether sulfonic acid （6∶2FTS）全氟己基乙烯基醚磺酸7.92427.0292.9349413C4-PFOA
386.929
406.8*23
13perfluorooctanoic acid （PFOA）全氟辛酸7.99413.1169.0173913C4-PFOA
219.016
369.0*10
14perfluoroheptanesulfonic acid （PFHpS）全氟庚烷磺酸8.01448.980.0*3812713C4-PFOA
99.038
169.033
15perfluorohexane sulfonamide （FHxSA）全氟己烷磺酰胺8.29398.078.0*289113C4-PFOS
169.027
377.921
16perfluorononanoic acid （PFNA）全氟壬酸8.41462.8219.0164213C5-PFNA
269.017
419.0*10
17perfluorooctanesulfonate （PFOS）全氟辛烷磺酸8.41498.980.0*4110913C4-PFOS
99.040
230.040
186∶2 chlorinated polyfluorinated ether sulfonate （6/2F-53B）6∶2氯代多氟烷基醚磺酸盐8.62531.0351.0*269713C2-PFDA
198∶2 fluorotelomer thioether amido sulfonate （8∶2FTS）8∶2氟代烷基硫醚酰胺磺酸盐8.72527.0392.93811013C2-PFDA
486.833
506.8*27
20perfluorodecanoic acid （PFDA）全氟癸酸8.73513.0219.0184513C2-PFDA
269.018
469.0*10
21perfluorononanoic acid （PFNS）全氟壬烷磺酸8.76549.180.0*4312513C2-PFDA
98.942
119.043
22N-methyl perfluorooctanesulfonamide （N-MeFOSAA）N-甲基全氟辛烷磺酰胺8.89570.0418.9*208613C5-PFNA
482.716
511.921
23N-ethyl perfluorooctane sulfonamido acetic acid （N-EtFOSAA）N-乙基全氟辛烷磺酰氨基乙酸9.03584.0418.9*207513C4-PFOA
482.916
525.920
24perfluoroundecanoic acid （PFUdA）全氟十一酸9.06563.1219.0185013C2-PFUdA
269.018
519.0*10
25perfluorodecanesulfonate （PFDS）全氟癸烷磺酸9.06598.980.0*4717513C2-PFUdA
99.045
26perfluorooctane sulfonamide （FOSA）全氟辛烷磺酰胺9.08498.078.0*3010518O2-PFHxS
429.713
477.925
2711-chloroperfluoro-3-oxaundecanesulfonic acid （11Cl-PF3OUDS）11-氯二十氟-3-氧杂十一烷-1-磺酸9.16631.035.2469313C2-PFDoA
450.9*29
468.923
288∶2 chlorinated polyfluorinated ether sulfonic acid （8/2F-53B）8∶2氯代多氟烷基醚磺酸盐9.20630.9450.9*2812213C4-PFOS
549.016
29perfluorododecanoic acid （PFDoA）全氟十二酸9.32613.1319.0185613C2-PFDoA
530.915
569.0*10
30perfluorotridecanoic acid （PFTrDA）全氟十三酸9.56663.1318.9195913C2-PFDoA
369.019
619.0*10
31perfluorotetradecanoic acid （PFTeDA）全氟十四酸9.76713.0318.9206213C2-PFDoA
630.917
669.0*10
32perfluoro-n-（1，2，3，4-13C4）butanoic acid （13C4-PFBA）13C4-全氟丁酸3.77217.019.25530
157.117
172.1*10
33perfluoro-n-（1，2-13C2） hexanoic acid （13C2-PFHxA）13C2-全氟己酸6.71315.091.01435
119.422
270.0*10
34sodiumperfluro-1-hexane（18O2）sulfonate （18O2-PFHxS）18O2-全氟己烷磺酸7.53403.084.0*36158
103.035
168.931
35perfluoro-n-（1，2，3，4-13C4）octanoic acid （13C4-PFOA）13C4-全氟辛酸7.94417.0172.11837
318.811
372.0*10
36perfluoro-n-（1，2，3，4，5-13C5）nonanoic acid （13C5-PFNA）13C5-全氟壬酸8.36468.0172.11941
218.817
422.8*10
37perfluoro-n-（1，2，3，4-13C4）octanesulfonate （13C4-PFOS）13C4-全氟辛烷磺酸8.36503.080.0*41100
99.041
111.027
38perfluoro-n-（1，2-13C2）decanoic acid （13C2-PFDA）13C2-全氟癸酸8.7515.1219.21851
269.418
470.0*12
39perfluoro-n-（1，2-13C2）undecanoic acid （13C2-PFUdA）13C2-全氟十一酸9.02565.3269.41842
319.318
520.1*10
40perfluoro-n-（1，2-13C2）dodecanoic acid （13C2-PFDoA）13C2-全氟十二酸9.32615.0319.31853
369.318
570.0*10
), ArticleFig(id=1322947230247825904, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, label=表1, caption=

31种PFASs和9种内标的保留时间和质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
No.CompoundChinese nameRT/minPrecursor ion （m/z）Product ion （m/z）CE/eVRF/VIS
1perfluorobutyric acid （PFBA）全氟丁酸3.77213.1169.0*103013C4-PFBA
180.810
182.817
2perfluorobutanesulfonate （PFBS）全氟丁烷磺酸盐6.02298.980.0*3310318O2-PFHxS
99.030
218.923
3sodium 1H，1H，2H，2H-perfluorohexane sulfonate（4∶2） （4∶2FTS）1H，1H，2H，2H-全氟己烷磺酸钠6.65327.080.4287713C4-PFBA
286.925
306.9*20
4perfluorohexanoic acid （PFHxA）全氟己酸6.78312.9119.1213013C2-PFHxA
269.0*10
295.217
5perfluoropentanesulfonic acid （PFPeS）全氟膦酸6.9349.180.0*3510518O2-PFHxS
99.032
119.033
6hexafluoropropylene oxide dimer acid （HFPO-DA）六氟环氧丙烷二聚酸6.93285.0119.0296213C2-PFHxA
169.0*10
185.019
7perfluorobutane sulfonamide （FBSA）全氟丁烷磺酰胺6.99298.078.0*257013C4-PFOA
119.019
218.819
8perfluoroheptanoic acid （PHHpA）全氟庚酸7.46362.9169.0173218O2-PFHxS
281.117
319.0*10
9sodium dodecafluoro-3H-4，8-dioxanonanoate （NaDONA）十二氟-3H-4，8-二氧六烯酸钠7.48377.085.0293813C4-PFOA
251.0*10
358.910
10dodecafluoro-3H-4，8-dioxanonane sodium salt （DONA）十二氟-3H-4，8-二氧杂壬酸钠7.53376.7250.9*104013C4-PFOA
11perfluorohexanesulfonate （PFHxS）全氟己烷磺酸7.53399.180.0*2311218O2-PFHxS
99.037
319.035
12perfluorohexyl ethyl vinyl ether sulfonic acid （6∶2FTS）全氟己基乙烯基醚磺酸7.92427.0292.9349413C4-PFOA
386.929
406.8*23
13perfluorooctanoic acid （PFOA）全氟辛酸7.99413.1169.0173913C4-PFOA
219.016
369.0*10
14perfluoroheptanesulfonic acid （PFHpS）全氟庚烷磺酸8.01448.980.0*3812713C4-PFOA
99.038
169.033
15perfluorohexane sulfonamide （FHxSA）全氟己烷磺酰胺8.29398.078.0*289113C4-PFOS
169.027
377.921
16perfluorononanoic acid （PFNA）全氟壬酸8.41462.8219.0164213C5-PFNA
269.017
419.0*10
17perfluorooctanesulfonate （PFOS）全氟辛烷磺酸8.41498.980.0*4110913C4-PFOS
99.040
230.040
186∶2 chlorinated polyfluorinated ether sulfonate （6/2F-53B）6∶2氯代多氟烷基醚磺酸盐8.62531.0351.0*269713C2-PFDA
198∶2 fluorotelomer thioether amido sulfonate （8∶2FTS）8∶2氟代烷基硫醚酰胺磺酸盐8.72527.0392.93811013C2-PFDA
486.833
506.8*27
20perfluorodecanoic acid （PFDA）全氟癸酸8.73513.0219.0184513C2-PFDA
269.018
469.0*10
21perfluorononanoic acid （PFNS）全氟壬烷磺酸8.76549.180.0*4312513C2-PFDA
98.942
119.043
22N-methyl perfluorooctanesulfonamide （N-MeFOSAA）N-甲基全氟辛烷磺酰胺8.89570.0418.9*208613C5-PFNA
482.716
511.921
23N-ethyl perfluorooctane sulfonamido acetic acid （N-EtFOSAA）N-乙基全氟辛烷磺酰氨基乙酸9.03584.0418.9*207513C4-PFOA
482.916
525.920
24perfluoroundecanoic acid （PFUdA）全氟十一酸9.06563.1219.0185013C2-PFUdA
269.018
519.0*10
25perfluorodecanesulfonate （PFDS）全氟癸烷磺酸9.06598.980.0*4717513C2-PFUdA
99.045
26perfluorooctane sulfonamide （FOSA）全氟辛烷磺酰胺9.08498.078.0*3010518O2-PFHxS
429.713
477.925
2711-chloroperfluoro-3-oxaundecanesulfonic acid （11Cl-PF3OUDS）11-氯二十氟-3-氧杂十一烷-1-磺酸9.16631.035.2469313C2-PFDoA
450.9*29
468.923
288∶2 chlorinated polyfluorinated ether sulfonic acid （8/2F-53B）8∶2氯代多氟烷基醚磺酸盐9.20630.9450.9*2812213C4-PFOS
549.016
29perfluorododecanoic acid （PFDoA）全氟十二酸9.32613.1319.0185613C2-PFDoA
530.915
569.0*10
30perfluorotridecanoic acid （PFTrDA）全氟十三酸9.56663.1318.9195913C2-PFDoA
369.019
619.0*10
31perfluorotetradecanoic acid （PFTeDA）全氟十四酸9.76713.0318.9206213C2-PFDoA
630.917
669.0*10
32perfluoro-n-（1，2，3，4-13C4）butanoic acid （13C4-PFBA）13C4-全氟丁酸3.77217.019.25530
157.117
172.1*10
33perfluoro-n-（1，2-13C2） hexanoic acid （13C2-PFHxA）13C2-全氟己酸6.71315.091.01435
119.422
270.0*10
34sodiumperfluro-1-hexane（18O2）sulfonate （18O2-PFHxS）18O2-全氟己烷磺酸7.53403.084.0*36158
103.035
168.931
35perfluoro-n-（1，2，3，4-13C4）octanoic acid （13C4-PFOA）13C4-全氟辛酸7.94417.0172.11837
318.811
372.0*10
36perfluoro-n-（1，2，3，4，5-13C5）nonanoic acid （13C5-PFNA）13C5-全氟壬酸8.36468.0172.11941
218.817
422.8*10
37perfluoro-n-（1，2，3，4-13C4）octanesulfonate （13C4-PFOS）13C4-全氟辛烷磺酸8.36503.080.0*41100
99.041
111.027
38perfluoro-n-（1，2-13C2）decanoic acid （13C2-PFDA）13C2-全氟癸酸8.7515.1219.21851
269.418
470.0*12
39perfluoro-n-（1，2-13C2）undecanoic acid （13C2-PFUdA）13C2-全氟十一酸9.02565.3269.41842
319.318
520.1*10
40perfluoro-n-（1，2-13C2）dodecanoic acid （13C2-PFDoA）13C2-全氟十二酸9.32615.0319.31853
369.318
570.0*10
), ArticleFig(id=1322947230327517681, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, label=Table 2, caption=

Regression equations， correlation coefficients （R2）， LODs， LOQs and recoveries （n=5） of the 31 PFASs

, figureFileSmall=null, figureFileBig=null, tableContent=
AnalyteRegression equationR2

LOD/

（pg/mL）

LOQ/

（pg/mL）

5 pg/mL5 ng/mL25 ng/mL
Recovery/%RSD/%Recovery/%RSD/%Recovery/%RSD/%
PFBAy=0.8248x+0.02110.9996258367.827.196.613.485.41.8
PFBSy=1.6518x‒0.00600.99950.0190.0661.710.7109.611.598.90.7
4∶2FTSy=0.4176x+0.00710.99980.010.03100.116.591.83.688.51.4
PFHxAy=1.1525x‒0.01070.99966.321140.37.2109.19.680.81.5
PFPeSy=1.0098x+0.00830.99990.210.7125.77.691.717.478.20.3
HFPO-DAy=0.0957x+0.00140.99810.391.3091.123.1106.918.299.82.2
FBSAy=0.6353x‒0.01230.99980.210.772.829.4105.613.197.21.7
PFHpAy=4.3409x‒0.04430.99942.68.7103.26.785.516.890.94.8
NaDONAy=1.5939x‒0.00980.99990.832.77102.63.279.113.190.15.5
PFHxSy=0.8123x+0.00630.99991.34.33139.321.695.314.588.70.6
6∶2FTSy=0.2976x+0.00380.99990.010.03120.725.8119.411.992.75.3
PFOAy=0.6552x+0.00350.99993.311195.419.592.513.696.94.6
PFHpSy=0.2650x+0.00070.99990.030.186.27.890.812.9119.31.8
FHxSAy=1.9626x‒0.01200.99970.581.9362.312.994.59.488.80.9
PFOSy=1.2570x+0.00900.99970.973.23199.15.4115.17.078.60.9
8/2F-53By=11.2170x‒0.07210.99970.190.63163.810.792.29.785.37.5
PFNAy=1.2058x‒0.01630.99932.27.33150.416.496.111.679.30.9
6/2F-53By=2.9025x‒0.02830.99990.571.9163.810.791.015.586.54.9
8∶2FTSy=0.3688x+0.00070.99980.0950.32110.39.8118.311.696.30.5
PFNSy=0.1777x+0.00200.99980.010.03150.416.496.814.476.20.1
N-MeFOSAAy=0.3315x‒0.00270.99940.882.93106.55.9109.711.7129.65.9
N-EtFOSAAy=0.2330x‒0.00090.99970.230.77143.916.995.822.2106.12.4
PFUdAy=0.7296x+0.00190.99990.62177.77.394.522.882.81.6
PFDSy=0.2290x+0.00020.99990.020.0761.66.690.59.479.70.6
FOSAy=0.5112x‒0.00850.99990.280.93102.922.998.412.992.21.2
PFDoAy=0.6711x‒0.00320.99951.34.3396.01.2107.511.585.31.7
PFTrDAy=0.6481x‒0.00210.99990.531.7795.89.992.412.181.53.2
PFDAy=0.8668x‒0.00500.99990.973.23158.714.897.012.781.41.0
PFTeDAy=0.9004x‒0.02070.99980.812.794.91.191.812.386.24.7
DONA1y=1.5079x‒0.00970.99991.75.6798.82.860.55.972.53.9
11Cl-PF3OUDSy=1.5204x‒0.00090.99990.120.469.28.180.616.874.50.5
), ArticleFig(id=1322947230411403762, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, label=表2, caption=

31种PFASs的回归方程、相关系数、检出限、定量限和加标回收率（n=5）

, figureFileSmall=null, figureFileBig=null, tableContent=
AnalyteRegression equationR2

LOD/

（pg/mL）

LOQ/

（pg/mL）

5 pg/mL5 ng/mL25 ng/mL
Recovery/%RSD/%Recovery/%RSD/%Recovery/%RSD/%
PFBAy=0.8248x+0.02110.9996258367.827.196.613.485.41.8
PFBSy=1.6518x‒0.00600.99950.0190.0661.710.7109.611.598.90.7
4∶2FTSy=0.4176x+0.00710.99980.010.03100.116.591.83.688.51.4
PFHxAy=1.1525x‒0.01070.99966.321140.37.2109.19.680.81.5
PFPeSy=1.0098x+0.00830.99990.210.7125.77.691.717.478.20.3
HFPO-DAy=0.0957x+0.00140.99810.391.3091.123.1106.918.299.82.2
FBSAy=0.6353x‒0.01230.99980.210.772.829.4105.613.197.21.7
PFHpAy=4.3409x‒0.04430.99942.68.7103.26.785.516.890.94.8
NaDONAy=1.5939x‒0.00980.99990.832.77102.63.279.113.190.15.5
PFHxSy=0.8123x+0.00630.99991.34.33139.321.695.314.588.70.6
6∶2FTSy=0.2976x+0.00380.99990.010.03120.725.8119.411.992.75.3
PFOAy=0.6552x+0.00350.99993.311195.419.592.513.696.94.6
PFHpSy=0.2650x+0.00070.99990.030.186.27.890.812.9119.31.8
FHxSAy=1.9626x‒0.01200.99970.581.9362.312.994.59.488.80.9
PFOSy=1.2570x+0.00900.99970.973.23199.15.4115.17.078.60.9
8/2F-53By=11.2170x‒0.07210.99970.190.63163.810.792.29.785.37.5
PFNAy=1.2058x‒0.01630.99932.27.33150.416.496.111.679.30.9
6/2F-53By=2.9025x‒0.02830.99990.571.9163.810.791.015.586.54.9
8∶2FTSy=0.3688x+0.00070.99980.0950.32110.39.8118.311.696.30.5
PFNSy=0.1777x+0.00200.99980.010.03150.416.496.814.476.20.1
N-MeFOSAAy=0.3315x‒0.00270.99940.882.93106.55.9109.711.7129.65.9
N-EtFOSAAy=0.2330x‒0.00090.99970.230.77143.916.995.822.2106.12.4
PFUdAy=0.7296x+0.00190.99990.62177.77.394.522.882.81.6
PFDSy=0.2290x+0.00020.99990.020.0761.66.690.59.479.70.6
FOSAy=0.5112x‒0.00850.99990.280.93102.922.998.412.992.21.2
PFDoAy=0.6711x‒0.00320.99951.34.3396.01.2107.511.585.31.7
PFTrDAy=0.6481x‒0.00210.99990.531.7795.89.992.412.181.53.2
PFDAy=0.8668x‒0.00500.99990.973.23158.714.897.012.781.41.0
PFTeDAy=0.9004x‒0.02070.99980.812.794.91.191.812.386.24.7
DONA1y=1.5079x‒0.00970.99991.75.6798.82.860.55.972.53.9
11Cl-PF3OUDSy=1.5204x‒0.00090.99990.120.469.28.180.616.874.50.5
), ArticleFig(id=1322947230482706931, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=EN, label=Table 3, caption=

Contents of PFASs in serum collected in first trimester of pregnancy women

, figureFileSmall=null, figureFileBig=null, tableContent=
CompoundDF/%Contents/（ng/mL）
MedianMeanMax
PFBA46-0.1461.27
PFBS900.1150.1140.315
4∶2FTS720.2470.8435.17
PFHxA760.0080.0890.523
PFPeS883.13.8414.0
HFPO-DA36-0.0580.31
FBSA4-0.0010.002
PFHpA38-0.0140.168
NaDONA48-0.0030.029
PFHxS905.635.3515.7
6∶2FTS641.252.9957.7
PFOA681.542.1812.3
PFHpS880.090.090.237
FHxSA8-0.0010.008
PFOS903.734.2812.6
8/2F-53B26-0.0020.003
PFNA900.4910.521.53
6/2F-53B901.091.307.71
8∶2FTS12-0.0491.21
PFNS880.0310.0300.091
N-MeFOSAA32-0.0040.033
N-EtFOSAA6-0.0010.031
PFUdA780.2720.3291.32
PFDS900.0260.0290.126
FOSA14-0.0010.015
PFDoA640.020.0320.15
PFTrDA32-0.0260.151
PFDA660.2890.5243.17
PFTeDA36-0.0050.059
11Cl-PF3OUDS8-0.0030.064
DONA34-0.0050.047
∑方正汇总行31PFASs21.822.973.9
), ArticleFig(id=1322947230566593012, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, language=CN, label=表3, caption=

孕妇孕早期血清中PFASs的含量

, figureFileSmall=null, figureFileBig=null, tableContent=
CompoundDF/%Contents/（ng/mL）
MedianMeanMax
PFBA46-0.1461.27
PFBS900.1150.1140.315
4∶2FTS720.2470.8435.17
PFHxA760.0080.0890.523
PFPeS883.13.8414.0
HFPO-DA36-0.0580.31
FBSA4-0.0010.002
PFHpA38-0.0140.168
NaDONA48-0.0030.029
PFHxS905.635.3515.7
6∶2FTS641.252.9957.7
PFOA681.542.1812.3
PFHpS880.090.090.237
FHxSA8-0.0010.008
PFOS903.734.2812.6
8/2F-53B26-0.0020.003
PFNA900.4910.521.53
6/2F-53B901.091.307.71
8∶2FTS12-0.0491.21
PFNS880.0310.0300.091
N-MeFOSAA32-0.0040.033
N-EtFOSAA6-0.0010.031
PFUdA780.2720.3291.32
PFDS900.0260.0290.126
FOSA14-0.0010.015
PFDoA640.020.0320.15
PFTrDA32-0.0260.151
PFDA660.2890.5243.17
PFTeDA36-0.0050.059
11Cl-PF3OUDS8-0.0030.064
DONA34-0.0050.047
∑方正汇总行31PFASs21.822.973.9
)], attaches=null, journal=Journal(id=1283839686691000338, delFlag=0, nameCn=色谱, nameEn=Chinese Journal of Chromatography, nameHistory1=null, nameHistory2=null, issn=1000-8713, eissn=null, cn=21-1185/O6, coden=SEPUER, periodic=0, language=CN, oaType=null, ccby=null, superviseOffice=null, ownerOffice=null, pubOffice=null, editorOffice=null, officeType=null, aims=null, clcCode=null, officeProv=null, officeCity=null, officeAddr=null, officeZip=null, officeEmail=null, officePhone=null, editDirector=null, officeDirector=null, officeDirectorPhone=null, officeStaffNum=null, officeEmpNum=null, coverPicUrl=TH9NrRkCT0gofr5swH2new==, journalPrice=null, startedYear=null, abbrevIsoEn=Chinese Journal of Chromatography, journalRemark=null, publicationField=null, createdTime=1784020833897, updatedTime=1788950977311, createdBy=18614031015, updatedBy=13041195026, firstLetterCn=S, firstLetterEn=S, subjectCode=Engineering, subjectName=null, subjectCodeEn=Engineering, subjectNameEn=null, picCn=TH9NrRkCT0gofr5swH2new==, picEn=A9oFBlfzKMJD115nwQwGog==, jcr=null, cjcr=null, exts=[JournalExt(id=1304518207025467898, language=CN, name=色谱, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1788950977331, updatedTime=1788950977331, createdBy=13041195026, updatedBy=13041195026, submissionGuidelinesUrl=, submissionAuthorUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionEditorUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionReviewUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1304518207159685627, language=EN, name=Chinese Journal of Chromatography, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1788950977363, updatedTime=1788950977363, createdBy=13041195026, updatedBy=13041195026, submissionGuidelinesUrl=, submissionAuthorUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionEditorUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionReviewUrl=https://mc03.manuscriptcentral.com/cjchrom, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1283840372199657495, websiteList=[Website(id=1283840757274493327, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1283840372199657495, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/sepu/CN, language=CN, createTime=1784021089142, createBy=18614031015, updateTime=1784023007420, updateBy=18614031015, name=色谱-中文, tplId=1146099689490845704, title=色谱, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1283849034246898091, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=articleTextType, value=kx, createTime=1784023062526, updateTime=1784023062526, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034217537960, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=banner, value=null, createTime=1784023062519, updateTime=1784023062519, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034272063918, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=grayFlag, value=0, createTime=1784023062532, updateTime=1784023062532, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034204955047, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=logo, value=https://castjournals.cast.org.cn/joweb/sepu/CN/file/pic?fileId=Wu//MG5V1kJkIhvqXIsmsw==, createTime=1784023062516, updateTime=1784023062516, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034280452528, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=minRunFlag, value=0, createTime=1784023062534, updateTime=1784023062534, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034230120874, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/sepu/CN/file/pic, createTime=1784023062522, updateTime=1784023062522, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034276258223, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=silenceFlag, value=0, createTime=1784023062533, updateTime=1784023062533, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034225926569, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1784023062521, updateTime=1784023062521, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034255286700, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=themeColor, value=null, createTime=1784023062528, updateTime=1784023062528, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849034263675309, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757274493327, code=themeStyle, value=null, createTime=1784023062530, updateTime=1784023062530, creator=18614031015, updator=18614031015)]), Website(id=1283840757333213590, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1283840372199657495, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/sepu/EN, language=EN, createTime=1784021089156, createBy=18614031015, updateTime=1784023028742, updateBy=18614031015, name=色谱-英文, tplId=1146101810881728533, title=Chinese Journal of Chromatography, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1283849003095802273, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=articleTextType, value=kx, createTime=1784023055099, updateTime=1784023055099, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003062247838, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=banner, value=null, createTime=1784023055091, updateTime=1784023055091, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003116773796, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=grayFlag, value=0, createTime=1784023055104, updateTime=1784023055104, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003049664925, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=logo, value=https://castjournals.cast.org.cn/joweb/sepu/EN/file/pic?fileId=Wu//MG5V1kJkIhvqXIsmsw==, createTime=1784023055088, updateTime=1784023055088, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003133551014, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=minRunFlag, value=0, createTime=1784023055108, updateTime=1784023055108, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003087413664, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/sepu/EN/file/pic, createTime=1784023055097, updateTime=1784023055097, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003125162405, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=silenceFlag, value=0, createTime=1784023055106, updateTime=1784023055106, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003074830751, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1784023055094, updateTime=1784023055094, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003104190882, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=themeColor, value=null, createTime=1784023055101, updateTime=1784023055101, creator=18614031015, updator=18614031015), WebsiteProps(id=1283849003108385187, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1283840757333213590, code=themeStyle, value=null, createTime=1784023055102, updateTime=1784023055102, creator=18614031015, updator=18614031015)])], journalTitle=色谱, weixinUrl=null, journalUrl=https://www.chrom-china.com/, iacademicId=null, status=1, seqNo=null, journalTitleEn=Chinese Journal of Chromatography, journalPhotoCn=TH9NrRkCT0gofr5swH2new==, journalPhotoEn=A9oFBlfzKMJD115nwQwGog==, journalFirstLetter=S, journalRecommend=null, journalNew=null, journalCollection=null, jcrJf=null, cjcrJf=null, jcrJfStr=null, cjcrJfStr=null, submissionFirstDecision=null, sciSubjectClassification=null, casSubjectClassification=null, citeScore=null, totalCitationFrequency=null, icpCode=null, psCode=null, advertisingLicenseCode=null, copyrightInformation=null, country=null, option=, provinceCode=null, provinceName=null, collectFlag=false, interPubPlatform=, interPubPlatformUrl=null), detailUrlCn=https://castjournals.cast.org.cn/joweb/sepu/CN/10.3724/SP.J.1123.2024.11028, detailUrlEn=https://castjournals.cast.org.cn/joweb/sepu/EN/10.3724/SP.J.1123.2024.11028, pdfUrlCn=https://castjournals.cast.org.cn/joweb/sepu/CN/PDF/10.3724/SP.J.1123.2024.11028, pdfUrlEn=https://castjournals.cast.org.cn/joweb/sepu/EN/PDF/10.3724/SP.J.1123.2024.11028, aliStartDate=0, aliEndDate=0, collectionFlag=false, citedCount=null, citedUrl=null, previewStatus=0, delFlag=0, hasFullText=1, orderTime=1751904000000, fullTextJson=null, articleText=null, reference=null)
收藏切换
冷冻诱导相分离结合液相色谱-串联质谱快速测定人血清中全氟和多氟烷基化合物
收藏切换
PDF下载
王建迪 1, 2 , 王仪伟 1 , 吴佳欣 1 , 施致雄 1, *
色谱 | 研究论文 2025,43(7): 756-766
收起
收藏切换
色谱 |研究论文 2025 , 43 (7) : 756 -766
冷冻诱导相分离结合液相色谱-串联质谱快速测定人血清中全氟和多氟烷基化合物
全屏
[Author(id=1322947224870728140, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947224958808527, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947224870728140, language=EN, stringName=Jiandi WANG, firstName=Jiandi, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, address=1. School of Public Health，Capital Medical University，Beijing 100069，China
2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225172718032, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947224870728140, language=CN, stringName=王建迪, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, 2, address=1.首都医科大学公共卫生学院，北京 100069
2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)]), AuthorCompany(id=1322947224765870536, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224782647753, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China), AuthorCompanyExt(id=1322947224795230666, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224765870536, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300)])]), Author(id=1322947225353073106, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=1, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947225428570580, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225353073106, language=EN, stringName=Yiwei WANG, firstName=Yiwei, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225491485141, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225353073106, language=CN, stringName=王仪伟, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])]), Author(id=1322947225554399703, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=2, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1322947225663451609, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225554399703, language=EN, stringName=Jiaxin WU, firstName=Jiaxin, middleName=null, lastName=WU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947225810252250, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225554399703, language=CN, stringName=吴佳欣, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])]), Author(id=1322947225927692764, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, orderNo=3, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=szx0127@ccmu.edu.cn, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1322947226179351007, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225927692764, language=EN, stringName=Zhixiong SHI, firstName=Zhixiong, middleName=null, lastName=SHI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1. School of Public Health，Capital Medical University，Beijing 100069，China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1322947226485535200, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, authorId=1322947225927692764, language=CN, stringName=施致雄, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1.首都医科大学公共卫生学院，北京 100069, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1322947224568738245, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, xref=null, ext=[AuthorCompanyExt(id=1322947224581321158, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. School of Public Health，Capital Medical University，Beijing 100069，China), AuthorCompanyExt(id=1322947224593904071, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322947109468635335, companyId=1322947224568738245, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.首都医科大学公共卫生学院，北京 100069)])])]
王建迪1, 2, 王仪伟1, 吴佳欣1, 施致雄1, *
作者信息
  • 1.首都医科大学公共卫生学院，北京 100069
  • 2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300
通讯作者:
Fast determination of per- and polyfluoroalkyl substances in human serum by cold-induced phase separation coupled with liquid chromatography-tandem mass spectrometry
Jiandi WANG1, 2, Yiwei WANG1, Jiaxin WU1, Zhixiong SHI1, *
Affiliations
  • 1. School of Public Health，Capital Medical University，Beijing 100069，China
  • 2. Shunyi Maternal and Children’s Hospital of Beijing Children’s Hospital，Beijing 101300，China
出版时间: 2025-07-08 doi: 10.3724/SP.J.1123.2024.11028
文章导航
收藏切换
摘要
收起

全氟和多氟烷基化合物（per- and polyfluoroalkyl substances， PFASs）的广泛应用带来了显著的环境污染与人群健康风险。血清测定是开展PFASs的人群内暴露评估及人群流行病学研究的基础，因此亟需建立可快速准确测定大规模人群血清中PFASs 的分析技术。本研究建立了可快速测定血清中31种PFASs的方法。血清中加入稳定性同位素内标后采用乙腈萃取，通过集净化与富集为一体的冷冻诱导相分离处理后，采用液相色谱-电喷雾电离-串联质谱在选择反应监测模式下采集质谱数据，内标法定量。对仪器分析参数和冷冻诱导相分离条件进行了优化。确定以乙腈为萃取溶剂，冷冻诱导相分离时溶液中乙腈体积分数为35%，-20 ℃下冷冻1 h为最佳样品前处理条件。在优化后的条件下，PFASs在0.5~20 ng/mL范围内线性良好，检出限为0.01~25 pg/mL，定量限为0.03~83 pg/mL；在5和25 ng/mL加标水平下，PFASs的平均回收率为60.5%~129.6%，相对标准偏差≤22.8%；在5 pg/mL定量限加标水平下，PFASs的平均回收率为61.6%~199.1%，RSD≤29.4%。采用所建立的方法测定了北京市顺义区50份孕妇血清样本，其中PFASs总和含量中值与均值分别为21.8和22.9 ng/mL，含量范围为0.456~73.9 ng/mL。有24种PFASs检出率在30%以上，其中9种检出率大于80%。高检出率表明PFASs的人群暴露普遍存在，同时胎儿可通过母-婴传递暴露于PFASs。此外传统PFASs和新型替代品检出率和污染水平均较高，人群暴露和潜在健康风险不容忽视。本研究所建立的方法操作简单，有机溶剂和耗材消耗极少，灵敏度和稳定性良好，适用于大规模人群监测与环境流行病学研究。

全氟和多氟烷基化合物  /  冷冻诱导  /  血清  /  同位素稀释  /  液相色谱-串联质谱

Per- and polyfluoroalkyl substances （PFASs） are a large group of synthetic chemicals that have been widely used in various industrial and commercial products owing to their unique physicochemical properties. However， accumulating evidence suggests that PFASs are persistent， transmissive over long distances， bioaccumulative， and toxic； consequently， their adverse effects on ecosystems and humans is of widespread concern. Serum is the most commonly used human matrix for assessing internal exposure to environmental pollutants， and several analytical methods have been developed to measure PFASs in sera. Current methods are generally fast， convenient， and robust； however， their pretreatment steps require large amounts of organic solvents and materials， such as solid-phase extraction cartridges and/or sorbents. In this study， a novel and low-cost analytical method based on cold-induced phase separation （CIPS） strategy was developed for the simultaneous determination of 31 legacy and emerging PFASs in serum. The core mechanism and distinctive feature of CIPS involves cooling an acetonitrile-water （ACN-water） mixture at a low temperature to produce two clear-cut layers： one with a high ACN proportion （the ACN layer） and an aqueous layer （water layer）. Certain chemicals are significantly enriched in the ACN layer during cooling； at the same time， impurities， especially water-soluble impurities， remain in the aqueous layer. CIPS only requires the temperature to be varied， and no external impurities are introduced during pretreatment， which dramatically reduces material costs and avoids new impurities from intervening. Our method involves the following procedure： serum was drawn accurately （0.2 mL） into a 1.5 mL Eppendorf （EP） tube， 2 ng of each isotopically labeled internal standard was added， the mixture is vortexed， and 350 µL of ACN was added， followed by vortexing and ultrasonic extraction. Subsequently， 450 µL of water is added to adjust the volume proportion of ACN to 35% （the volume percentage of ACN in the total solution）. The protein at the bottom of the tube was collected following centrifugation at 15 000 r/min for 10 min， and the supernatant was transferred to a 1 mL syringe. The syringe was frozen in a -20 ℃ refrigerator for 1 h to obtain the two layers， after which the upper layer （approximately 80–100 μL） containing ACN and the target compounds was finally transferred to a glass vial for instrumental analysis. Liquid chromatography coupled with triple quadrupole mass spectrometry augmented with electrospray ionization （LC-ESI-MS/MS） was used to quantify the PFASs. The analytes were separated using a C18 column， with methanol and 2 mmol/L of ammonium formate-H2O used as mobile phases. Linearities， limits of detection （LODs） and， limits of quantification （LOQs）， recoveries， precisions， and matrix effects were determined under the optimal conditions. The LODs and LOQs of PFASs in serum were 0.01–25 and 0.03–83 pg/mL， respectively. Under two spiked levels， namely 5 ng/mL and 25 ng/mL， average recoveries ranged between 60.5% and 129.6%， with relative standard deviations （RSDs） of less than 22.8%. Under 5 pg/mL as LOD spiked level， average recoveries ranged between 61.6% and 199.1%，with RSDs<29.4%. While matrix-effect testing revealed slightly enhanced signals， the use of isotopically labeled internal standards compensated for these effects. Real samples were subsequently analyzed， with 50 human serum samples collected in first trimester of pregnancy women living in the Shunyi District， Beijing. Nine PFASs exhibited high detection frequencies （>80%）， which suggests that PFASs are ubiquitous in the population. The median and mean levels of Σ31PFASs （sum of 31 PFASs） in serum were 21.8 and 22.9 ng/mL， respectively， and the range was 0.456-73.9 ng/mL. Both legacy and emerging PFASs were detected at high frequencies and contamination levels， which suggests that they are widely used. In summary， the method developed in this study is fast， sensitive， and solvent- and material-efficient； it is also very linear and highly accurate， and exhibits satisfactory extraction recovery and enrichment factors； hence， it is suitable for surveying large populations as well as for use in environmental epidemiology.

per- and polyfluoroalkyl substances （PFASs）  /  cold-induced  /  serum  /  isotope dilution  /  liquid chromatography-tandem mass spectrometry （LC-MS/MS）
王建迪, 王仪伟, 吴佳欣, 施致雄. 冷冻诱导相分离结合液相色谱-串联质谱快速测定人血清中全氟和多氟烷基化合物. 色谱, 2025 , 43 (7) : 756 -766 . DOI: 10.3724/SP.J.1123.2024.11028
Jiandi WANG, Yiwei WANG, Jiaxin WU, Zhixiong SHI. Fast determination of per- and polyfluoroalkyl substances in human serum by cold-induced phase separation coupled with liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2025 , 43 (7) : 756 -766 . DOI: 10.3724/SP.J.1123.2024.11028
正文
收起
全氟和多氟烷基化合物（per- and polyfluoroalkyl substances，PFASs）是一类含有高能碳氟（C-F）共价键的小分子化合物的统称，由于性质稳定并具有特殊的疏水和疏油性，被广泛应用于工业生产和各类民用产品中，但PFASs的生产、使用和产品废弃过程也带来了环境污染以及生态健康风险［1］。体内外实验已表明，PFASs具有遗传、生殖、神经和发育毒性，以及内分泌干扰作用和疑似致癌性［2］。PFASs同时具有难降解，以及在环境中呈现持久性和生物富集性等特点，是国际公认的“永久性化合物（forever chemicals）”［1，3］。全氟辛酸（pefluorooctanic acid， PFOA）和全氟辛烷磺酸 （perfluorooctane sulfonate， PFOS）等部分PFASs已被列入《关于持久性有机污染物的斯德哥尔摩公约》中，但由于难以找到合适的替代品，已使用多年的一些传统全氟化合物仍在使用。同时，近年来作为替代品的一些多氟类化合物的使用量在迅速上升，由此带来的人群暴露与健康风险亟待明确。血清是评估环境污染物人群内暴露特征并开展环境流行病学研究的主要基质［4］，现有研究已开发出若干种测定血清中PFASs的方法。由于挥发性较弱，PFASs的仪器分析以液相色谱-串联质谱法为主［5，6］。在前处理方面，目前多采用固相萃取法［7，8］或基质固相分散萃取法［9］进行样本处理与净化，也有研究采用离子对液液萃取法［10］。现有前处理方法具有快速简便、稳定可靠且处理通量高等优点，但缺点是需消耗大量昂贵试剂和耗材。冷冻诱导相分离技术（cold-induced phase separation，CIPS）是近期发展起来的一种快速、简便、低成本的前处理技术［11，12］，其核心原理是使用乙腈萃取待测化合物后，加入适量水混合成适当比例的乙腈-水混合物，随后低温冷冻促进相分离形成乙腈层和水层，在相分离过程中特定化合物会显著富集至乙腈层，同时杂质尤其是水溶性杂质会保留在水层中。相分离后乙腈层可直接取出进行液相色谱-质谱分析。CIPS的显著优势是仅需极少量有机溶剂，且无需使用固相萃取柱或吸附剂等昂贵耗材，大大降低了前处理成本，同时最大限度地避免了前处理过程中外来杂质的引入。本研究结合CIPS和液相色谱-串联质谱法，建立了血清中31种PFASs的同时前处理与定量方法，并用于孕妇血清样本的测定，为开展PFASs的大规模人群流行学研究提供技术支持。
1 实验部分
收起
1.1 仪器、试剂与材料
UltiMate 3000型高效液相色谱仪、TSQ Altis Quantum Ultra三重四极杆质谱仪（美国Thermo Fisher Scientific公司）；5430 R型高速冷冻离心机（德国Eppendorf公司）。
31种PFASs标准溶液和9种同位素内标标准溶液均购自天津阿尔塔科技有限公司，纯度高于98%（表1），用甲醇稀释配制成合适浓度的混合标准工作液及内标混合工作液。实验用水为超纯水（Milli-Q纯水仪，美国默克公司）；甲酸铵、甲醇和乙腈均为色谱纯（美国Thermo Fisher Scientific公司）；用于方法验证实验的胎牛血清购自上海ExCell Bio公司。实际血清样本来自北京市顺义区妇幼保健院所建立的“顺义妇幼健康之约”队列，所有血清捐献者已被明确告知队列研究目的并签署知情同意书。本研究已获得顺义区妇幼保健院医学伦理委员会审查通过（审编号2024-021-2）。
1.2 样品前处理
取含内标50 pg/μL的内标混合工作液40 μL于1.5 mL 离心管中，氮气吹干溶液中的甲醇后加入200 μL血清样品并涡旋振荡1 min；加入350 μL乙腈，再次涡旋振荡1 min，随后超声萃取20 min；加入纯水450 μL，涡旋30 s后在15 000 r/min下离心10 min；取上清液转移至1 mL一次性注射器（7.2 cm×0.5 cm）中，于直立状态下置于-20 ℃冰箱中冷冻1 h后，在保持冷冻分层状态下迅速使用长型玻璃巴斯德吸管吸取上层液体（80~100 μL），转移至带玻璃内插管的进样小瓶中待上机检测。前处理过程中避免使用聚四氟乙烯材质的器皿以控制外源性污染。
1.3 液相色谱-质谱条件
Shim-pack GISS-HP C18色谱柱（150 mm×2.1 mm，3 μm，日本岛津公司）；流动相：A相为2 mmol/L甲酸铵水溶液，B相为甲醇，流速0.4 mL/min。柱温箱温度35 ℃，进样体积5 μL。梯度洗脱程序：0~0.5 min，20%B；0.5~9 min，20%B~100%B；9~12 min，100%B；12~15 min，20%B。
离子源：电喷雾电离源（ESI），负离子模式；电喷雾电压2 500 V；离子传输线温度325 ℃；气化温度350 ℃。以氮气作为鞘气和辅助气，流速分别设置为50和10 Arb；数据采集模式：选择反应监测模式（SRM）。31种PFASs的质谱分析参数及每种PFASs对应内标如表1所示。
1.4 萃取回收率和富集系数计算方法
采用萃取回收率（Rec.）和富集系数（enrichment factor，EF）评价CIPS萃取并富集PFASs的效率。萃取回收率定义为相分离后乙腈层中待测物质量与原始样本液中的质量之比。富集系数定义为乙腈层中待测物浓度（Cu）与原始样本溶液中的浓度（Ci）之比。计算公式如下：
Rec.=(Cu×Vu)/(Ci×Vi)
EF=Cu/Ci
式中， Vu和Vi分别为相分离后乙腈层的体积（依据注射器刻度测量）和原始样本液体积。
2 结果与讨论
收起
2.1 仪器分析条件的优化
使用各PFASs标准溶液进行全扫描，确定各目标物的保留时间以及母离子和产物离子，每个化合物确定一对定量离子对和至少两对定性离子对。由于部分PFASs尤其是新型多氟化合物尚未有商品化同位素内标，需与其他化合物共用内标。依据待测物与内标需物理化学性质近似，且保留时间与质谱响应相近的原则，结合加标回收结果优选出各待测物最适宜的内标物。对碰撞能量、离子源温度、传输线温度、梯度程序等条件进行优化，使31种PFASs最大程度上实现分离且达到最佳响应，获得的最优质谱参数见表1，混合标准溶液的总离子流色谱图如图1所示。
2.2 样品前处理条件的优化
2.2.1 CIPS前处理步骤简介
CIPS前处理大致分为3个步骤。首先使用有机溶剂进行液液或固液萃取提取待测物。乙腈可有效提取各类不同极性的有机物，是最常用的提取溶剂，本实验中乙腈在萃取PFASs的同时还能有效沉淀并通过离心除去血清中的蛋白质。第二步是向萃取液中加入适量水以调节乙腈在溶液中的比例（由于血清基本成分为水，因此实验中0.2 mL血清也视为0.2 mL水）。第三步是在适宜温度和时间下冷冻诱导相分离。第三步是CIPS的独特特征，其核心原理是合适比例的乙腈-水混合物在低温下可相分离形成乙腈层和水层，在相分离过程中特定化合物会显著富集至乙腈层，同时杂质尤其是水溶性杂质保留在水层中。相分离后乙腈层可直接取出进行液相色谱-质谱分析。
2.2.2 相分离时溶液中乙腈比例的优化
在冷冻诱导相分离过程中，溶液中乙腈占总体积的比例是影响待测物回收率和富集系数的主要因素。通常随着乙腈比例的降低，乙腈层体积也会缩小，同时富集系数会提高，直至乙腈比例下降至冷冻诱导相分离无法发生为止［13］。本研究以胎牛血清作为模拟物，通过对胎牛血清加标样品（10 ng/mL）的测定探索最优乙腈比例。在维持血清（0.2 mL）-乙腈-水混合液总体积为1 mL的前提下，通过改变所加入乙腈和水的体积，探索不同乙腈比例下PFASs的富集系数和萃取回收率。实验中观察到当乙腈比例（乙腈体积占溶液总体积的比例）低于30%时相分离难以发生，而当乙腈比例过高（大于70%）时冷冻后乙腈层体积过大，不利于待测物的富集，因此较佳的乙腈比例应控制为30%~70%。随后探索了乙腈比例从35%上升至70%时各待测物的富集系数和萃取回收率（见图2）。所有PFASs的富集系数随着乙腈比例的上升均呈现显著的下降趋势（图2a），尤其是乙腈比例从35%上升到40%时，富集系数下降幅度达50%以上，说明当乙腈比例控制在35%时PFASs能更有效地富集至乙腈层，而随着乙腈比例的上升，乙腈层体积增大导致其中待测物浓度显著降低，不利于待测物的仪器分析。从萃取回收率来看（图2b），随着乙腈比例的上升，大部分PFASs（PFBA、PFBS、PFHxA、PFPeS、PFHxS、PFOA、PFOS、8/2F-53B、PFNA、PFUdA、PFDS、PFDoA、PFDA等）的回收率均在100%左右且无剧烈变动，说明这些化合物及其内标物在相分离过程中无论乙腈比例如何变化，均能稳定地富集到乙腈层中。另有部分化合物在低乙腈比例（35%~40%）下具有较好的回收率，但随着乙腈比例的增高有变差的趋势，包括FBSA、6/2F-53B、N-MeFOSAA、N-EtFOSAA、PFTeDA、11Cl-PF3OUDS等。综合考虑，为满足大部分PFASs的准确测定，本研究决定控制冷冻诱导相分离时的乙腈比例为35%，即溶液中乙腈为350 μL，水为650 μL。
2.2.3 冷冻诱导温度和时间的优化
除了乙腈比例，冷冻诱导温度和时间也会影响相分离。通常低温可促进相分离，当乙腈比例控制在35%时，发现在超低温（-80 ℃）条件下，溶液在几分钟内便会迅速冻结，导致乙腈和水无法分离。在-40 ℃条件下冷冻40 min后形成清晰稳定的乙腈层和水层。在-20 ℃冰箱中也能形成清晰稳定的乙腈层和水层，但冷冻时间需在1 h以上，时间过短会导致相分离不完全并影响待测物富集和水相中蛋白质沉淀。但如果冷冻时间过久，容易在乙腈层中形成絮状冰晶影响后续乙腈层的吸取转移。考虑到-20 ℃冰箱更为常用，建议在溶液总体积为1 mL时，冷冻诱导以-20 ℃冷冻1 h为宜。
2.3 方法验证
2.3.1 标准曲线与检出限
配制系列标准溶液，标准溶液中PFASs的质量浓度分别为0.5、1、5、10和20 ng/mL，内标均为5 ng/mL。以各PFASs与相应内标的峰面积之比作为纵坐标（y），PFASs与相应内标的浓度之比作为横坐标（x），得到各目标物的标准曲线和相关系数（R2）。结果显示，各PFASs在0.5~20 ng/mL范围内线性良好，相关系数均大于0.99（表2）。以3倍信噪比计算方法的检出限（LOD），10倍信噪比计算方法的定量限（LOQ），PFASs的LOD为0.01~25 pg/mL，LOQ为0.03~83 pg/mL（表2）。
2.3.2 加标回收试验
以胎牛血清作为加标基质，设定定量限（5 pg/mL，本研究中PFASs的平均定量限）、低（5 ng/mL）和高（25 ng/mL）3个加标水平开展加标回收试验（表2）。在定量限加标回收试验中，各化合物的平均加标回收率为61.6%~199.1%，RSD≤29.4%。部分化合物，例如PFOA和PFOS，在极低的加标量下受血清和试剂耗材中存在的背景污染干扰严重，导致加标回收率偏高。而某些新型PFASs，例如PFDS、8/2F-53B和N-EtFOSAA，由于没有对应的同位素内标，导致加标回收率偏高或偏低。在低和高加标回收试验中，各化合物的平均加标回收率分别为60.5%~119.6%（RSD≤22.8%）和72.5%~129.6%（RSD≤7.5%）。加标回收实验结果表明本方法具有较好的回收率和精密度。
2.4 基质效应
虽然前处理过程中可将生物基质中的蛋白质和脂肪等大部分杂质通过沉淀方式除去［14］，但残存的一些杂质仍有可能在质谱分析中抑制或增强待测物响应。为评估前处理后残存杂质对目标物定量的影响，本研究用建立的前处理方法对血清样品进行前处理，获得空白基质溶液。将标准工作液分别添加到空白基质溶液和甲醇中以达到相同的加标水平，制备基质匹配溶液和试剂标准溶液并进行LC-MS/MS测定。以基质匹配溶液和试剂标准溶液中各待测物峰面积比评估基质效应。该比值<0.5或>1.5表示基质效应强烈，体现为显著抑制或增强［15］。本实验计算了待测物在5 ng/mL和50 ng/mL两个加标水平下的基质效应，结果显示在血清样中各PFASs均呈现出较弱的基质增强效应（比值范围1.1~1.5）。但随着待测物浓度的降低，基质效应出现增强趋势。通常，基质增强效应由杂质中某些可增强离子化效率的成分引起。在基质效应实验中，不同加标水平下，待测物浓度降低的同时溶液中杂质含量并未改变，因此低浓度加标液中的待测物受增强离子化效率的影响更严重，导致低浓度加标样本出现基质效应更强的趋势。虽然仅观察到较弱的基质效应，但在PFASs的检测中稳定性同位素内标的使用依然必不可少。
2.5 实际样品测定
已有动物实验表明孕期PFASs暴露可显著影响胎体生长发育［16］，因此亟需明确大规模人群孕期PFASs暴露水平，以便开展人群流行病学研究。本研究使用已建立的方法测定了孕妇孕早期（<孕13周）血清样本50份（表3）。有24种PFASs在血清中检出率在30%以上，其中9种检出率在80%以上。高检出率表明PFASs的人群暴露普遍存在，同时胎儿可通过母-婴传递暴露于PFASs。血清中PFASs总和含量中值与均值分别为21.8和22.9 ng/mL，含量范围为0.456~73.9 ng/mL。血清含量水平较高的依然是PFHxS、PFPeS、PFOA和PFOS等传统PFASs，但部分新型替代品如6/2F-53B和6∶2FTS也具有很高的检出率和含量，表明目前市场上传统和新型PFASs均存在大量使用的现象，人群暴露和潜在健康风险不容忽视。
3 结论
收起
本研究基于冷冻诱导相分离技术结合液相色谱-串联质谱法建立了血清中多种PFASs同时前处理与定量的分析技术。该方法操作简单，可节省大量有机溶剂及耗材，并具有较好的准确度和精密度，适用于大规模人群的内暴露监测。
基金
收起
  • 首都卫生发展科研专项（首发2022-2G-4264）
  • 首都卫生发展科研专项(2024-2G-7103)
  • 北京市教育委员会科技计划重点项目(KZ20231002549)
  • 北京市高层次公共卫生技术人才建设项目(2023-03-46)
文献
收起
参考文献 引证文献
排序方式：
1
Wang Y W， Zhang Q R， Yu N Y， et al. Progress in Chemistry， 2024， 36（11）： 1607
王亚韡， 张秋瑞， 于南洋， 等. 化学进展， 2024， 36（11）： 1607
2
Xing W Y， Sun J N， Liu F H， et al. J Hazard Mater， 2024， 472： 134556
3
Criswell R， Fleisch A F， Ducatman A. JAMA， 2024， 332（10）： 785
4
Zhang M Y， Cao Y， Li X， et al. Chinese Journal of Chromatography， 2024， 42（2）： 217
张明烨， 曹衍， 李想， 等. 色谱， 2024， 42（2）： 217
5
Feng H， Zhang W， He B S， et al. Chinese Journal of Chromatography， 2024， 42（8）： 731
冯灏， 张炜， 何保山， 等. 色谱， 2024， 42（8）： 731
6
Liu X Q， Liu Z Z， Wang M Y， et al. Chinese Journal of Chromatography， 2024， 42（8）： 740
刘小琦， 刘真真， 王美玉， 等. 色谱， 2024， 42（8）： 740
7
Lin Q， Wang J， Li J J， et al. Chinese Journal of Chromatography， 2024， 43（3）： 252
林强， 王健， 李晶晶， 等. 色谱， 2024， 43（3）： 252
8
Wang Z， Zhang B Y， Zhang J M， et al. Journal of Environmental and Occupational Medicine， 2024， 41（4）： 375
王铮， 张博雅， 张济明， 等. 环境与职业医学， 2024， 41（4）： 375
9
Xiao K T， Zhang B N， Wang Y C， et al. Environmental Chemistry， 2025. DOI： 10.7524/j.issn.0254-6108.2024022102
肖锴婷， 张博钠， 王祎纯， 等. 环境化学， 2025. DOI： 10.7524/j.issn.0254-6108.2024022102
10
Xie L N， Zhang H J， Hou S S， et al. Journal of Environmental Hygiene， 2019， 9（5）： 494
谢琳娜， 张海婧， 侯沙沙， 等. 环境卫生学杂志， 2019， 9（5）： 494
11
Liu Z， Chen D， Lyu B， et al. Anal Chem， 2022， 94（10）： 4227
12
Wu J， Yao S， Wang Y， et al. Anal Bioanal Chem， 2024， 416（28）： 6663
13
Li S， Ren J， Zhang Y， et al. Food Chem， 2020， 328： 127113
14
Shao G， Agar J， Giese R W. J Chromatog A， 2017， 1506： 128
15
Qi P P， Wang J， Liu Z Z， et al. J Chromatogr A， 2021， 1659： 462589
16
Guo C H， Fan Y S， Qiao Y Z， et al. Progress in Veterinary Medicine， 2020， 41（12）： 120
郭聪慧， 范玉珊， 乔延召， 等. 动物医学进展， 2020， 41（12）： 120
2025年第43卷第7期
PDF下载
33
15
引用本文
BibTeX
文章信息
doi: 10.3724/SP.J.1123.2024.11028
  • 接收时间：2024-12-14
  • 首发时间：2026-10-30
  • 出版时间：2025-07-08
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期：2024-12-14
基金
Capital’s Funds for Health Improvement and Research（CFH，2022-2G-4264）
首都卫生发展科研专项（首发2022-2G-4264）
Capital’s Funds for Health Improvement and Research(2024-2G-7103)
首都卫生发展科研专项(2024-2G-7103)
R&D Program of Beijing Municipal Education Commission(KZ20231002549)
北京市教育委员会科技计划重点项目(KZ20231002549)
Talent Development Plan for High-level Public Health Technical Personnel Project in Beijing(2023-03-46)
北京市高层次公共卫生技术人才建设项目(2023-03-46)
作者信息
    1.首都医科大学公共卫生学院，北京 100069
    2.北京市顺义区妇幼保健院，北京儿童医院顺义妇儿医院，北京 101300

通讯作者:

参考文献
分享链接
https://castjournals.cast.org.cn/joweb/sepu/CN/10.3724/SP.J.1123.2024.11028
分享至
全文二维码

扫描看全文

引用本文
BibTeX
本文的引用情况
2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
关闭全屏
相关链接
论文
最新文章
热读文章
热点专题
内参
蓝皮书
产业发展报告
传播力报告
期刊分级目录
资讯
学术新闻
行业新闻
学术会议
行业会议
关于
关于我们
联系我们
北京市海淀区学院南路86号
100081
010-62662699（运营及技术支持）
qkjq@cast.org.cn

中国科学技术协会版权所有 京ICP 备10216604号-4 海淀分局备案 1101084647
科技导报社主办 中国科协信息中心技术支持