Article(id=1322945534864007561, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945494665797748, articleNumber=null, orderNo=null, doi=10.3724/SP.J.1123.2024.10018, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1730304000000, receivedDateStr=2024-10-31, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793344394651, onlineDateStr=2026-10-30, pubDate=1757260800000, pubDateStr=2025-09-08, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793344394651, onlineIssueDateStr=2026-10-30, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793344394651, creator=13701087609, updateTime=1793344394651, updator=13701087609, issue=Issue{id=1322945494665797748, tenantId=1146029695717560320, journalId=1283840372199657495, year='2025', volume='43', issue='9', pageStart='987', pageEnd='1085', issueExtLink='null', onlineDate='null', pubDate='1757260800000', pubDateStr='2025-09-08', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793344385067, creator='13701087609', updateTime=1793345219786, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322948995802334087, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945494665797748, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322948995802334088, tenantId=1146029695717560320, journalId=1283840372199657495, issueId=1322945494665797748, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1063, endPage=1069, ext={EN=ArticleExt(id=1322945535237300618, articleId=1322945534864007561, tenantId=1146029695717560320, journalId=1283840372199657495, language=EN, title=Rapid determination of five antipyretic analgesics in surface water by online solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry, columnId=1284557502633185292, journalTitle=Chinese Journal of Chromatography, columnName=Articles, runingTitle=null, highlight=null, articleAbstract=
Antipyretic analgesics are typical pharmaceutical and personal care products （PPCPs） that are widely used in our daily life because they relieve fever and pain， and have anti-inflammatory and anti-rheumatic properties. These drugs inhibit the synthesis and release of prostaglandins （PGs） in the neurons of the anterior hypothalamus and exert therapeutic effects as a consequence. However， these drugs are relatively commonly misused and abused， often owing to a lack of proper medication guidance. As a result， these drugs enter the environment via various pathways， including wastewater treatment plants， agricultural runoff， and improper disposal， thereby posing potential threats to human health and ecosystems. The presence of these contaminants in surface water has become an environmental safety concern that necessitates the development of rapid， accurate， and high-throughput analysis methods. In this study， an analytical method was established for the determination of five antipyretic analgesics （ibuprofen， aminophenazone， antipyrine， phenacetin， and naproxen）. The developed method is based on online solid phase extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry （online SPE-UHPLC-MS/MS）， which provides a high degree of automation and efficiency. Water samples were collected and filtered through 0.2-μm regenerated cellulose （RC） filter membranes， after which Na2EDTA and an internal standard were added. An aliquot （0.9 mL） of each sample was injected into the online SPE system using an automatic sampler. Samples were first adsorbed on a PLRP-S online SPE column， washed with 0.05% formic acid aqueous solution， and finally gradient-eluted with a mobile phase composed of 0.2 mmol/L ammonium fluoride solution and methanol-acetonitrile （1∶1， v/v）. Analytes were separated on a ZORBAX Eclipse Plus C18 column， detected by multiple reaction monitoring with electrospray ionization in both positive- and negative-ion modes， and quantified using the internal-standard method.The five antipyretic analgesics were effectively separated under the optimized experimental conditions and showed good linearities within their respective concentration ranges， with correlation coefficients （r） greater than 0.998. The method detection limits （MDLs） ranged from 0.05 to 0.20 ng/L， and the method quantification limits （MQLs） ranged from 0.20 to 0.80 ng/L. The five antipyretic analgesics exhibited average recoveries of between 64.2% and 112%， with relative standard deviations （RSDs， n=6） of 2.06%-8.99% at low， medium， and high spiked levels. Furthermore， the method was successfully used to analyze water samples from the Hangzhou section of the Qiantang River， in which four target compounds were detected， with antipyrine found to have the highest mass concentration. This newly developed method features a high degree of automation， facilitates the injection of large volumes， and enables online enrichment， purification， and quantitative analysis in an integrated process， with minimal operational errors， high repeatability， and high sensitivity. The developed method shortens sample-analysis times， is more cost-effective， and meets the needs of large-scale sample testing， as it requires only 15 min to completely determine a sample， thereby significantly improving detection efficiency. Overall， the method features low detection limits， analyzes rapidly， and is easy to operate； hence it is suitable for rapid risk screening and the quantitative determination of antipyretic analgesics in surface water.
, authors=Ping HE
1, Liqun WANG
1, Shan ZHOU
1, Baofeng ZHANG
1, Xuan JIA
1, Yi CHI
1, Zhenqi XU
1, Wei TANG
2, *, authorsList=Ping HE, Liqun WANG, Shan ZHOU, Baofeng ZHANG, Xuan JIA, Yi CHI, Zhenqi XU, Wei TANG, authorCompany=null, correspAuthors=Wei TANG, 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=1322945538190090643, articleId=1322945534864007561, tenantId=1146029695717560320, journalId=1283840372199657495, language=CN, title=在线固相萃取-超高效液相色谱-串联质谱法快速测定地表水中5种解热镇痛药物, columnId=1284557502792568846, journalTitle=色谱, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
布洛芬等解热镇痛药物在日常生活中被广泛应用，其残留物可通过多种途径进入环境，对人类健康和生态环境具有潜在威胁。基于在线固相萃取-超高效液相色谱-串联质谱技术（online SPE-UHPLC-MS/MS），建立了一种快速筛查和检测地表水中布洛芬、氨基比林、安替比林、非那西丁和萘普生等5种常用解热镇痛药物的方法。样品经0.2 µm再生纤维素滤膜过滤，移取5 mL并加入一定量的内标和Na2EDTA，混匀，使用在线固相萃取系统自动上样，PLRP-S在线固相萃取柱富集净化。利用ZORBAX Eclipse Plus C18色谱柱（100 mm×3.0 mm，1.8 µm）进行分离，以甲醇-乙腈（1∶1，v/v）和0.2 mmol/L氟化铵水溶液为流动相进行梯度洗脱，采用电喷雾离子源，正、负离子扫描模式和多反应监测（MRM）模式检测，内标法定量。结果显示，采用该方法，5种解热镇痛药物在各自的线性范围内线性关系良好（r>0.998），方法检出限（MDL）为0.05~0.20 ng/L，方法定量限（MQL）为0.20~0.80 ng/L，在低、中、高3个加标水平下的回收率为64.2%~112%，相对标准偏差为2.06%~8.99%。采用该方法对取自钱塘江杭州段的6份水样进行检测，除氨基比林外，其余4种解热镇痛药物均有检出。该方法实现了大体积进样、在线富集净化及定量分析，简化了前处理步骤，15 min即可完成一个样品的测定，显著提高了检测效率，具有低检出限、高灵敏度、快速分析和操作简便的特点，适用于地表水中5种解热镇痛药物的快速测定。
, authors=何平
1, 王立群
1, 周姗
1, 张宝锋
1, 贾璇
1, 池怡
1, 徐珍琪
1, 唐伟
2, *, authorsList=何平, 王立群, 周姗, 张宝锋, 贾璇, 池怡, 徐珍琪, 唐伟, authorCompany=null, correspAuthors=唐伟, authorNote=null, correspAuthorsNote=
, 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
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Hangzhou Institute of Ecological Environment Science （Hangzhou Urban Ecological Environment Monitoring Station），Hangzhou 310014，China), AuthorCompanyExt(id=1322946778508701802, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, companyId=1322946778491924584, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.杭州市生态环境科学研究院 （杭州市城区生态环境监测站），浙江 杭州 310014)])], figs=[ArticleFig(id=1322946781205639324, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Fig. 1, caption=
Chromatograms of the target compounds with different chromatographic columns, figureFileSmall=kKRecVCD1H6NDKl3KoPCiw==, figureFileBig=7Tsk8pev2/funKnRWnD4DQ==, tableContent=null), ArticleFig(id=1322946782849806493, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=图1, caption=
采用不同色谱柱时目标化合物的色谱图, figureFileSmall=kKRecVCD1H6NDKl3KoPCiw==, figureFileBig=7Tsk8pev2/funKnRWnD4DQ==, tableContent=null), ArticleFig(id=1322946782946275486, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Fig. 2, caption=
Chromatograms of the target compounds under different aqueous phasesOrganic phase： methanol-acetonitrile （1∶1， v/v）.
, figureFileSmall=YGUpqdKdUYVwXSKRg426cg==, figureFileBig=xnhc8lfiDFWxwLT0YhzyNA==, tableContent=null), ArticleFig(id=1322946783009190047, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=图2, caption=
目标化合物在不同水相体系下的色谱图, figureFileSmall=YGUpqdKdUYVwXSKRg426cg==, figureFileBig=xnhc8lfiDFWxwLT0YhzyNA==, tableContent=null), ArticleFig(id=1322946783076298912, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Fig. 3, caption=
Effect of different filter membranes on the recoveries of the target compounds （n=3）RC： regenerated cellulose； PVDF： polyvinylidene fluoride； PTFE： polytetrafluoroethylene； PES： polyethersulfone； GHP： polypropylene.
, figureFileSmall=BTr//hRfOIlDUEQz6ZFYLA==, figureFileBig=fNTebMhyu/rJSZXdNHx4ZA==, tableContent=null), ArticleFig(id=1322946783151796385, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=图3, caption=
不同滤膜材质对目标化合物回收率的影响 （n=3）, figureFileSmall=BTr//hRfOIlDUEQz6ZFYLA==, figureFileBig=fNTebMhyu/rJSZXdNHx4ZA==, tableContent=null), ArticleFig(id=1322946783214710946, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Fig. 4, caption=
Chromatograms of the target compounds with different rinsing solventsFA： formic acid.
, figureFileSmall=gFleKt2/shAQ/tjU1/6Gpw==, figureFileBig=I/QO2Gfjvq9xL1gSvcAOZg==, tableContent=null), ArticleFig(id=1322946783294402723, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=图4, caption=
采用不同淋洗溶剂时目标化合物的色谱图, figureFileSmall=gFleKt2/shAQ/tjU1/6Gpw==, figureFileBig=I/QO2Gfjvq9xL1gSvcAOZg==, tableContent=null), ArticleFig(id=1322946783357317284, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Table 1, caption=
Gradient elution conditions of online solid phase extraction （online SPE）
, figureFileSmall=null, figureFileBig=null, tableContent=
| Time/min | Flow rate/（mL/min） | φ（Ａ）/% | φ（B）/% |
|---|
| 0 | 0.40 | 100 | 0 |
| 0.25 | 1.00 | 100 | 0 |
| 4.00 | 1.00 | 100 | 0 |
| 5.00 | 1.00 | 0 | 100 |
| 10.00 | 1.00 | 0 | 100 |
| 10.01 | 1.00 | 100 | 0 |
| 13.00 | 1.00 | 100 | 0 |
| 15.00 | 0.40 | 100 | 0 |
), ArticleFig(id=1322946783428620453, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=表 1, caption=
在线固相萃取梯度洗脱条件
, figureFileSmall=null, figureFileBig=null, tableContent=
| Time/min | Flow rate/（mL/min） | φ（Ａ）/% | φ（B）/% |
|---|
| 0 | 0.40 | 100 | 0 |
| 0.25 | 1.00 | 100 | 0 |
| 4.00 | 1.00 | 100 | 0 |
| 5.00 | 1.00 | 0 | 100 |
| 10.00 | 1.00 | 0 | 100 |
| 10.01 | 1.00 | 100 | 0 |
| 13.00 | 1.00 | 100 | 0 |
| 15.00 | 0.40 | 100 | 0 |
), ArticleFig(id=1322946783495729318, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Table 2, caption=
Retention times and MS parameters of the target compounds
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Retention time/min | Precursor ion （m/z） | Product ions （m/z） | Fragmentor/V | Collision energies/eV | Ionization mode |
|---|
| Ibuprofen （IBU） | 12.181 | 205.0 | 161.1* | 83 | 5， 5 | ESI- |
| Atipyrine （ANT） | 7.822 | 189.0 | 77.0*， 147.0 | 90 | 30， 20 | ESI+ |
| Aminophenazone （APZ） | 8.189 | 232.0 | 113.0*， 111.0 | 100 | 12， 10 | ESI+ |
| Phenacetin （PCT） | 8.797 | 180.1 | 65.1*， 110.0 | 118 | 55， 40 | ESI- |
| Naproxen （NPX） | 10.729 | 229.0 | 169.0*， 185.0 | 23 | 36， 2 | ESI- |
| Ibuprofen-D3 （IBU-D3） | 12.166 | 208.0 | 164.1* | 85 | 5， 5 | ESI- |
), ArticleFig(id=1322946783567032487, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=表 2, caption=
目标化合物的保留时间与质谱参数
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Retention time/min | Precursor ion （m/z） | Product ions （m/z） | Fragmentor/V | Collision energies/eV | Ionization mode |
|---|
| Ibuprofen （IBU） | 12.181 | 205.0 | 161.1* | 83 | 5， 5 | ESI- |
| Atipyrine （ANT） | 7.822 | 189.0 | 77.0*， 147.0 | 90 | 30， 20 | ESI+ |
| Aminophenazone （APZ） | 8.189 | 232.0 | 113.0*， 111.0 | 100 | 12， 10 | ESI+ |
| Phenacetin （PCT） | 8.797 | 180.1 | 65.1*， 110.0 | 118 | 55， 40 | ESI- |
| Naproxen （NPX） | 10.729 | 229.0 | 169.0*， 185.0 | 23 | 36， 2 | ESI- |
| Ibuprofen-D3 （IBU-D3） | 12.166 | 208.0 | 164.1* | 85 | 5， 5 | ESI- |
), ArticleFig(id=1322946783629947048, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Table 3, caption=
Linear ranges， regression equations， correlation coefficients （r）， MDLs， and MQLs of the target compounds
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Linear range/（ng/L） | Regression equation | r | MDL/（ng/L） | MQL/（ng/L） |
|---|
| IBU | 1.0-100 | y=1.48x+0.32 | 0.9985 | 0.20 | 0.80 |
| ANT | 0.5-100 | y=3.53x-0.13 | 0.9995 | 0.05 | 0.20 |
| APZ | 0.5-100 | y=10.89x-0.75 | 0.9996 | 0.09 | 0.36 |
| PCT | 0.5-100 | y=4.85x-0.17 | 0.9995 | 0.11 | 0.44 |
| NPX | 0.5-100 | y=2.10x-0.15 | 0.9989 | 0.05 | 0.20 |
), ArticleFig(id=1322946783709638825, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=表 3, caption=
目标化合物的线性范围、回归方程、相关系数、方法检出限及方法定量限
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Linear range/（ng/L） | Regression equation | r | MDL/（ng/L） | MQL/（ng/L） |
|---|
| IBU | 1.0-100 | y=1.48x+0.32 | 0.9985 | 0.20 | 0.80 |
| ANT | 0.5-100 | y=3.53x-0.13 | 0.9995 | 0.05 | 0.20 |
| APZ | 0.5-100 | y=10.89x-0.75 | 0.9996 | 0.09 | 0.36 |
| PCT | 0.5-100 | y=4.85x-0.17 | 0.9995 | 0.11 | 0.44 |
| NPX | 0.5-100 | y=2.10x-0.15 | 0.9989 | 0.05 | 0.20 |
), ArticleFig(id=1322946783768359082, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Table 4, caption=
Recoveries and RSDs of the target compounds at three spiked levels （n=6）
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Added/（ng/L） | Recovery/% | RSD/% |
|---|
| IBU | 2.0 | 86.0 | 4.87 |
| 10.0 | 103 | 8.99 |
| 50.0 | 112 | 2.06 |
| ANT | 2.0 | 93.5 | 6.58 |
| 10.0 | 100 | 5.62 |
| 50.0 | 89.4 | 4.07 |
| APZ | 2.0 | 90.1 | 4.30 |
| 10.0 | 74.1 | 3.61 |
| 50.0 | 70.8 | 2.77 |
| PCT | 2.0 | 103 | 2.98 |
| 10.0 | 69.1 | 2.17 |
| 50.0 | 64.2 | 4.08 |
| NPX | 2.0 | 98.8 | 5.76 |
| 10.0 | 89.9 | 4.21 |
| 50.0 | 103 | 4.54 |
), ArticleFig(id=1322946783827079339, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=表 4, caption=
目标化合物在3个加标水平下的平均回收率及相对标准偏差（n=6）
, figureFileSmall=null, figureFileBig=null, tableContent=
| Compound | Added/（ng/L） | Recovery/% | RSD/% |
|---|
| IBU | 2.0 | 86.0 | 4.87 |
| 10.0 | 103 | 8.99 |
| 50.0 | 112 | 2.06 |
| ANT | 2.0 | 93.5 | 6.58 |
| 10.0 | 100 | 5.62 |
| 50.0 | 89.4 | 4.07 |
| APZ | 2.0 | 90.1 | 4.30 |
| 10.0 | 74.1 | 3.61 |
| 50.0 | 70.8 | 2.77 |
| PCT | 2.0 | 103 | 2.98 |
| 10.0 | 69.1 | 2.17 |
| 50.0 | 64.2 | 4.08 |
| NPX | 2.0 | 98.8 | 5.76 |
| 10.0 | 89.9 | 4.21 |
| 50.0 | 103 | 4.54 |
), ArticleFig(id=1322946783894188204, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=EN, label=Table 5, caption=
Detection results of the five antipyretic analgesics in actual water samples
, figureFileSmall=null, figureFileBig=null, tableContent=
| Sample No. | IBU | ANT | APZ | PCT | NPX |
|---|
| 1 | ND | 5.0 | ND | ND | ND |
| 2 | ND | 0.4 | ND | ND | 1.1 |
| 3 | ND | 1.4 | ND | 0.5 | 2.4 |
| 4 | ND | ND | ND | ND | ND |
| 5 | ND | 16.3 | ND | 0.4 | 1.6 |
| 6 | 2.0 | 13.7 | ND | ND | 2.4 |
), ArticleFig(id=1322946783957102765, tenantId=1146029695717560320, journalId=1283840372199657495, articleId=1322945534864007561, language=CN, label=表 5, caption=
实际水样中5种解热镇痛药物的检测结果 (ng/L)
, figureFileSmall=null, figureFileBig=null, tableContent=
| Sample No. | IBU | ANT | APZ | PCT | NPX |
|---|
| 1 | ND | 5.0 | ND | ND | ND |
| 2 | ND | 0.4 | ND | ND | 1.1 |
| 3 | ND | 1.4 | ND | 0.5 | 2.4 |
| 4 | ND | ND | ND | ND | ND |
| 5 | ND | 16.3 | ND | 0.4 | 1.6 |
| 6 | 2.0 | 13.7 | ND | ND | 2.4 |
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