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Article(id=1324078533064131470, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1324078333767594037, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202508373, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1755878400000, receivedDateStr=2025-08-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793614522471, onlineDateStr=2026-11-02, pubDate=1767974400000, pubDateStr=2026-01-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793614522471, onlineIssueDateStr=2026-11-02, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793614522471, creator=13701087609, updateTime=1793614522471, updator=13701087609, issue=Issue{id=1324078333767594037, tenantId=1146029695717560320, journalId=1227665162245664772, year='2026', volume='53', issue='1', pageStart='1', pageEnd='192', issueExtLink='null', onlineDate='null', pubDate='1767974400000', pubDateStr='2026-01-10', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1793614474956, creator='13701087609', updateTime=1793614571752, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1324078739914621270, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1324078333767594037, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1324078739914621271, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1324078333767594037, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=154, endPage=159, ext={EN=ArticleExt(id=1324078533278040975, articleId=1324078533064131470, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Simultaneous determination of seven parabens in beef tallow hotpot seasoning by QuEChERS-gas chromatography-mass spectrometry, columnId=1228016572065837304, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish a QuEChERS-gas chromatography-mass spectrometry method for the simultaneous determination of seven parabens in beef tallow hotpot seasoning.

Methods

To an accurately weighed quantity of the homogenized sample, water, the internal standard and acetronitrile were added, and the analytes were extracted and purified by QuEChERS, analyzed by gas chromatography-mass spectrometry and quantified by internal standard method.

Results

Good linearity was observed for all seven analytes over the range of 0.05 to 5.00 μg/mL, with r≥0.999. The limits of detection (LODs) were between 0.05 and 0.06 mg/kg, and the limits of quantitation (LOQs) were between 0.15 and 0.20 mg/kg.The average recoveries of the method were between 91.4% and 108%, with the relative standard deviations (RSDs) between 0.6% and 7.2%.

Conclusion

The method is simple, accurate and sensitive, and is suitable for the simultaneous determination of seven parabens in beef tallow hotpot seasoning.

, authors=Chang-xiao YANG1, Kun ZHANG1, Yong-yang ZHOU2, authorsList=Chang-xiao YANG, Kun ZHANG, Yong-yang ZHOU, authorCompany=null, correspAuthors=Kun ZHANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, 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=1324078536033698711, articleId=1324078533064131470, tenantId=1146029695717560320, journalId=1227665162245664772, language=CN, title=QuEChERS-气相色谱-质谱法同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂, columnId=1228016572288135432, journalTitle=现代预防医学, columnName=实验技术及其应用, runingTitle=null, highlight=null, articleAbstract=
目的

建立同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的QuEChERS-气相色谱-质谱法。

方法

称取一定量均质化样品，加入水、内标物和乙腈，经QuEChERS法提取、净化后，气相色谱-质谱法分析，内标法定量。

结果

在0.05～5.00 μg/ml范围内，七种被测物均呈现良好的线性关系，相关系数均大于0.999；检出限和定量限分别为0.05～0.06 mg/kg和0.15～0.20 mg/kg；平均加标回收率为91.4%～108%，相对标准偏差为0.6%～7.2%。

结论

本方法操作方便、准确、灵敏，适用于牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的测定。

, authors=杨长晓1, 张坤1, 周永杨2, authorsList=杨长晓, 张坤, 周永杨, authorCompany=null, correspAuthors=张坤, authorNote=

杨长晓(1983—)，男，本科，副主任技师，研究方向：食品理化检验

, correspAuthorsNote=
张坤，E-mail:
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(In Chinese), articleTitle=null, refAbstract=null), Reference(id=1324078549514191845, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, doi=null, pmid=null, pmcid=null, year=2025, volume=16, issue=7, pageStart=55, pageEnd=62, url=null, language=null, rfNumber=[24], rfOrder=40, authorNames=陈锂, 张恺, 杨杭, journalName=食品安全质量检测学报, refType=null, unstructuredReference=陈锂，张恺，杨杭，等.QuEChERS-气相色谱-串联三重四极杆质谱法测定食用油中7种抗氧化剂残留[J].食品安全质量检测学报，2025，16（7）：55-62., articleTitle=QuEChERS-气相色谱-串联三重四极杆质谱法测定食用油中7种抗氧化剂残留, refAbstract=null), Reference(id=1324078549631632358, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, doi=null, pmid=null, pmcid=null, year=2025, volume=16, issue=7, pageStart=55, pageEnd=62, url=null, language=null, rfNumber=[24], rfOrder=41, authorNames=Chen L, Zhang K, Yang H, journalName=Journal of Food Safety & Quality, refType=null, unstructuredReference=Chen L, Zhang K, Yang H, et al. 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Determination of 14 kinds of fluorescent whitening agents in hot pot condiment by QuEChERS-Ultra high performance liquid Chromatography-Tandem mass spectrometry[J]. Food Science and Technology, 2025, 50(3): 329-337. (In Chinese), articleTitle=Determination of 14 kinds of fluorescent whitening agents in hot pot condiment by QuEChERS-Ultra high performance liquid Chromatography-Tandem mass spectrometry, refAbstract=null), Reference(id=1324078549883290601, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, doi=null, pmid=null, pmcid=null, year=2022, volume=28, issue=9, pageStart=133, pageEnd=136, 144, url=null, language=null, rfNumber=[26], rfOrder=44, authorNames=燕群, 党翠红, 张育, journalName=现代食品, refType=null, unstructuredReference=燕群，党翠红，张育.气相色谱法测定食品中4种对羟基苯甲酸酯类含量[J].现代食品，2022，28（9）：133-136, 144., articleTitle=气相色谱法测定食品中4种对羟基苯甲酸酯类含量, refAbstract=null), Reference(id=1324078549950399466, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, doi=null, pmid=null, pmcid=null, year=2022, volume=28, issue=9, pageStart=133, pageEnd=136, 144, url=null, language=null, rfNumber=[26], rfOrder=45, authorNames=Yan Q, Dang CH, Zhang Y, journalName=Modern Food, refType=null, unstructuredReference=Yan Q, Dang CH, Zhang Y. 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Determination of 6 parabens in Soy sauce by QuEChERS purification GC-MS/MS[J]. Sichuan Food and Fermentation, 2023, 59(4): 151-155. (In Chinese), articleTitle=Determination of 6 parabens in Soy sauce by QuEChERS purification GC-MS/MS, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1324078536729953176, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, xref=1., ext=[AuthorCompanyExt(id=1324078536742536089, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, companyId=1324078536729953176, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Sichuan Center for Disease Control and Prevention, Chengdu, Sichuan 610041, China), AuthorCompanyExt(id=1324078536750924698, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, companyId=1324078536729953176, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.四川省疾病预防控制中心，四川 成都 610041)]), AuthorCompany(id=1324078536826422171, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, xref=2., ext=[AuthorCompanyExt(id=1324078536839005084, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, companyId=1324078536826422171, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.达州市疾病预防控制中心)])], figs=[ArticleFig(id=1324078541033309109, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=EN, label=Figure 1, caption=Total ion chromatograms (TIC) of a mixed standard solution and a blank sample spiked solution, figureFileSmall=vViS/CkYQWsI7FeBqkHzBw==, figureFileBig=HJXN0QlWz78SrP0bv9xW1g==, tableContent=null), ArticleFig(id=1324078541339493302, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=CN, label=图1, caption=混合标准溶液、及空白样品加标溶液、的总离子谱图

注：峰号为1—MeP；2—EtP + EtP-D4；3—Iso-PrP；4—PrP；5—Iso-BuP；6—BuP；7—HeP；A为混合标准溶液（1.00 μg/ml)；B为空白样品加标溶液（5.00 mg/kg）。

, figureFileSmall=vViS/CkYQWsI7FeBqkHzBw==, figureFileBig=HJXN0QlWz78SrP0bv9xW1g==, tableContent=null), ArticleFig(id=1324078541859586999, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=EN, label=Table 1, caption=

GC-MS analysis parameters of parabens

, figureFileSmall=null, figureFileBig=null, tableContent=
中文名称英文名称（缩写）保留时间（min）定量离子（m/z）定性离子（m/z）
对羟基苯甲酸甲酯methyl paraben（MeP）8.446121152、93
对羟基苯甲酸乙酯ethyl paraben（EtP）8.889121138、166
D4-对羟基苯甲酸乙酯ethyl paraben-D4 (EtP-D4)8.889125170
对羟基苯甲酸异丙酯isopropyl paraben（Iso-Prp）9.071121138、180
对羟基苯甲酸丙酯propyl paraben（Prp）9.504121138、180
对羟基苯甲酸异丁酯isobutyl paraben（Iso-BuP）9.848121138、194
对羟基苯甲酸丁酯butyl paraben（BuP）10.111121138、194
对羟基苯甲酸庚酯heptyl paraben（HeP）11.725121138、139
), ArticleFig(id=1324078541947667384, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=CN, label=表1, caption=

对羟基苯甲酸酯类化合物的GC-MS分析参数

, figureFileSmall=null, figureFileBig=null, tableContent=
中文名称英文名称（缩写）保留时间（min）定量离子（m/z）定性离子（m/z）
对羟基苯甲酸甲酯methyl paraben（MeP）8.446121152、93
对羟基苯甲酸乙酯ethyl paraben（EtP）8.889121138、166
D4-对羟基苯甲酸乙酯ethyl paraben-D4 (EtP-D4)8.889125170
对羟基苯甲酸异丙酯isopropyl paraben（Iso-Prp）9.071121138、180
对羟基苯甲酸丙酯propyl paraben（Prp）9.504121138、180
对羟基苯甲酸异丁酯isobutyl paraben（Iso-BuP）9.848121138、194
对羟基苯甲酸丁酯butyl paraben（BuP）10.111121138、194
对羟基苯甲酸庚酯heptyl paraben（HeP）11.725121138、139
), ArticleFig(id=1324078542161576889, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=EN, label=Table 2, caption=

Regression equations, correlation coefficient, limit of detection (LOD) and limit of quantitation (LOQ)

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物回归方程相关系数（r）检出限（mg/kg）定量限（mg/kg）
MePy=1.733x-0.1560.999 90.050.15
EtPy =1.983x-0.1490.999 90.050.15
Iso-PrPy=1.984x-0.2910.999 90.050.15
PrPy=1.834x-0.4250.999 60.050.15
Iso-BuPy=1.906x-0.5430.999 60.050.15
BuPy=1.614x-0.4890.999 60.050.15
HePy=1.033x-0.0740.999 70.060.20
), ArticleFig(id=1324078542249657274, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=CN, label=表2, caption=

回归方程、相关系数、检出限和定量限

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物回归方程相关系数（r）检出限（mg/kg）定量限（mg/kg）
MePy=1.733x-0.1560.999 90.050.15
EtPy =1.983x-0.1490.999 90.050.15
Iso-PrPy=1.984x-0.2910.999 90.050.15
PrPy=1.834x-0.4250.999 60.050.15
Iso-BuPy=1.906x-0.5430.999 60.050.15
BuPy=1.614x-0.4890.999 60.050.15
HePy=1.033x-0.0740.999 70.060.20
), ArticleFig(id=1324078542329349051, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=EN, label=Table 3, caption=

Recovery and precision determination results (n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物加标水平（mg/kg）测定值[mg/kg，（）]平均回收率（%）相对标准偏差（%）
MeP0.3000.285±0.01795.25.7
5.0005.100±0.100102.02.0
20.00019.500±0.10097.50.6
EtP0.3000.295±0.01198.53.7
5.0005.310±0.220106.04.2
20.00020.100±0.300101.01.5
Iso-PrP0.3000.293±0.00996.63.1
5.0004.870±0.17097.43.5
20.00020.400±0.500102.02.4
PrP0.3000.301±0.014102.04.6
5.0005.380±0.060108.01.1
20.00019.100±0.20095.50.8
Iso-BuP0.3000.298±0.01993.26.3
5.0004.800±0.14096.02.9
20.00020.000±0.500100.02.7
BuP0.3000.288±0.01494.34.9
5.0005.040±0.150101.03.0
20.00019.30±0.40096.52.1
HeP0.3000.290±0.02192.77.2
5.0004.570±0.24091.45.3
20.00019.700±0.70098.53.8
), ArticleFig(id=1324078542409040828, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1324078533064131470, language=CN, label=表3, caption=

回收率和精密度测定结果（n=6）

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物加标水平（mg/kg）测定值[mg/kg，（）]平均回收率（%）相对标准偏差（%）
MeP0.3000.285±0.01795.25.7
5.0005.100±0.100102.02.0
20.00019.500±0.10097.50.6
EtP0.3000.295±0.01198.53.7
5.0005.310±0.220106.04.2
20.00020.100±0.300101.01.5
Iso-PrP0.3000.293±0.00996.63.1
5.0004.870±0.17097.43.5
20.00020.400±0.500102.02.4
PrP0.3000.301±0.014102.04.6
5.0005.380±0.060108.01.1
20.00019.100±0.20095.50.8
Iso-BuP0.3000.298±0.01993.26.3
5.0004.800±0.14096.02.9
20.00020.000±0.500100.02.7
BuP0.3000.288±0.01494.34.9
5.0005.040±0.150101.03.0
20.00019.30±0.40096.52.1
HeP0.3000.290±0.02192.77.2
5.0004.570±0.24091.45.3
20.00019.700±0.70098.53.8
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QuEChERS-气相色谱-质谱法同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂
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杨长晓 1 , 张坤 1 , 周永杨 2
现代预防医学 | 实验技术及其应用 2026,53(1): 154-159
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现代预防医学 |实验技术及其应用 2026 , 53 (1) : 154 -159
QuEChERS-气相色谱-质谱法同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂
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杨长晓1, 张坤1 , 周永杨2
作者信息
  • 1.四川省疾病预防控制中心，四川 成都 610041
  • 2.达州市疾病预防控制中心
通讯作者:
张坤，E-mail:
作者简介:

杨长晓(1983—)，男，本科，副主任技师，研究方向：食品理化检验

Simultaneous determination of seven parabens in beef tallow hotpot seasoning by QuEChERS-gas chromatography-mass spectrometry
Chang-xiao YANG1, Kun ZHANG1 , Yong-yang ZHOU2
Affiliations
  • Sichuan Center for Disease Control and Prevention, Chengdu, Sichuan 610041, China
出版时间: 2026-01-10 doi: 10.20043/j.cnki.MPM.202508373
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摘要
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目的

建立同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的QuEChERS-气相色谱-质谱法。

方法

称取一定量均质化样品，加入水、内标物和乙腈，经QuEChERS法提取、净化后，气相色谱-质谱法分析，内标法定量。

结果

在0.05～5.00 μg/ml范围内，七种被测物均呈现良好的线性关系，相关系数均大于0.999；检出限和定量限分别为0.05～0.06 mg/kg和0.15～0.20 mg/kg；平均加标回收率为91.4%～108%，相对标准偏差为0.6%～7.2%。

结论

本方法操作方便、准确、灵敏，适用于牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的测定。

牛油火锅底料  /  对羟基苯甲酸酯  /  QuEChERS  /  气相色谱-质谱法
Objective

To establish a QuEChERS-gas chromatography-mass spectrometry method for the simultaneous determination of seven parabens in beef tallow hotpot seasoning.

Methods

To an accurately weighed quantity of the homogenized sample, water, the internal standard and acetronitrile were added, and the analytes were extracted and purified by QuEChERS, analyzed by gas chromatography-mass spectrometry and quantified by internal standard method.

Results

Good linearity was observed for all seven analytes over the range of 0.05 to 5.00 μg/mL, with r≥0.999. The limits of detection (LODs) were between 0.05 and 0.06 mg/kg, and the limits of quantitation (LOQs) were between 0.15 and 0.20 mg/kg.The average recoveries of the method were between 91.4% and 108%, with the relative standard deviations (RSDs) between 0.6% and 7.2%.

Conclusion

The method is simple, accurate and sensitive, and is suitable for the simultaneous determination of seven parabens in beef tallow hotpot seasoning.

Beef tallow hotpot seasoning  /  Parabens  /  QuEChERS  /  Gas chromatography-mass spectrometry
杨长晓, 张坤, 周永杨. QuEChERS-气相色谱-质谱法同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂. 现代预防医学, 2026 , 53 (1) : 154 -159 . DOI: 10.20043/j.cnki.MPM.202508373
Chang-xiao YANG, Kun ZHANG, Yong-yang ZHOU. Simultaneous determination of seven parabens in beef tallow hotpot seasoning by QuEChERS-gas chromatography-mass spectrometry[J]. Modern Preventive Medicine, 2026 , 53 (1) : 154 -159 . DOI: 10.20043/j.cnki.MPM.202508373
正文
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对羟基苯甲酸酯类化合物（parabens，又名尼泊金酯）具备高效广谱的抑菌性能，因而被广泛用作饮料、调味品等各类食品的防腐剂[1]。牛油火锅底料是川渝地区极具特色的调味品，消费频次高且受众群体广泛。豆瓣酱等原料可能在牛油火锅底料的生产过程中引入对羟基苯甲酸酯类防腐剂[2]，人为添加和环境代入也可能导致此类食品中检出对羟基苯甲酸酯类化合物[3]。近年来，对羟基苯甲酸酯类防腐剂的安全性引发持续争议。多项研究证实，长期过量摄入该类物质可能导致人体内分泌紊乱，诱发皮肤黏膜过敏等健康问题，其中儿童、孕妇等敏感群体面临的健康风险尤为显著[4-7]，甚至有研究发现对羟基苯甲酸酯类化合物和乳腺癌存在一定的关联[8]。因此，有必要建立一种快速、准确的测定牛油火锅底料中对羟基苯甲酸酯类防腐剂的方法，为食品安全监管提供技术支撑。
多项研究证实对羟基苯甲酸酯类化合物联合使用可产生显著的协同抑菌效应[9]，但因为分子结构的差别，不同酯型的潜在健康风险并不一致[10]，因此并非所有对羟基苯甲酸酯类化合物均可作为食品防腐剂使用。我国仅允许对羟基苯甲酸甲酯和乙酯作为防腐剂在部分食品中使用[11]，同时明确规定对羟基苯甲酸丙酯不能用作食品添加剂[12]。基于此，通常情况下需要此类物质分别进行检测以保障食品安全。目前，针对食品中对羟基苯甲酸酯类防腐剂的检测，气相色谱法（gas chromatography,GC）[13]、高效液相色谱法（high performance liquid chromatography，HPLC）[14]、气相色谱-质谱法（GC-mass spectrometry，GC-MS）[15]、气相色谱-串联质谱法（GC-tandem mass spectrometry，GC-MS/MS）[16]、液相色谱-串联质谱法（liquid chromatography-tandem mass spectrometry,LC-MS/MS）[17-18]、超高效液相色谱-高分辨质谱法（ultra-high performance liquid chromatography-high resolution mass spectrometry，UPLC-HRMS）[19]等均有报道。《食品安全国家标准 食品中对羟基苯甲酸酯类化合物的测定》（GB 5009.31—2025）也规定了GC、HPLC和LC-MS/MS等方法用于测定不同类型食品中的对羟基苯甲酸酯类防腐剂[20]。这些方法中，GC和HPLC的定性能力有限，面对复杂基质样品时易出现假阳性结果，而GC-MS/MS、LC-MS/MS和UPLC-HRMS法所需设备价格昂贵，在国内基层实验室尚未普及，难以广泛应用；相比较之下，GC-MS法能满足定性需求，且仪器经济适用，基层普及率高。另外，这些方法主要集中于酱油、醋、果汁等样品基质，针对牛油火锅底料中该类防腐剂的检测方法尚未见报道。
牛油火锅底料是一种以牛油为主要油脂来源，融合辣椒、花椒、姜、蒜、八角、桂皮等多种香辛料，搭配豆瓣酱、豆豉、冰糖等调味成分熬制而成的特色调味品[21]，其基质中高比例的油脂易包裹目标物而导致提取效率偏低；同时，香辛料中含有的色素、挥发油及酚类物质，会与目标物在色谱分离中产生共流出峰，干扰定性定量，增加假阳性风险。
QuEChERS技术具备高效性、经济性和普适性等优势，在食品中农药残留的快速检测领域应用广泛[22-23]；近年来，该技术的应用范围进一步拓展，已有报道显示其可用于食品中抗氧化剂[24]、荧光增白剂[25]等其它类型污染物检测的样品前处理环节。本研究采用QuEChERS技术进行目标物的提取和净化，并采用GC-MS对目标物进行分离检测。该方法不仅有效解决了传统方法定性能力不足及基体干扰严重等问题，还具备灵敏度高、准确性好、操作简便的优势，为牛油火锅底料中对羟基苯甲酸酯类防腐剂的检测提供了可靠方案。
1　材料与方法
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1.1　材料与试剂
七种对羟基苯甲酸酯混合标准溶液（1 000 μg/ml）、D4-对羟基苯甲酸乙酯标准溶液（1 000 μg/ml）购于北京曼哈格生物技术有限公司；乙腈（色谱纯）购于德国Sigma公司；陶瓷均质子、ProElut QuE En萃取盐包（含NaCl、MgSO4、柠檬酸钠、柠檬酸氢二钠，分别为1、4、1和0.5 g）和ProElut QuE 15 ml净化管（含C18、PSA、GCB、MgSO4，分别为400、400、200和1 200 mg）购于北京迪马科技有限公司；尼龙66膜过滤器（0.22 μm）购于湖南比克曼控股有限公司；实验用水为超纯水。牛油火锅底料样品，购于本地超市和粮油干杂店。
1.2　主要仪器与设备
7890A/7000C气相色谱-质谱仪（Agilent Technologies，美国)，H2100R高速冷冻离心机（上海卢湘仪离心机仪器有限公司），Multi Reax涡旋振荡器（Heidolph，德国），HM100刀式研磨仪（北京格瑞德曼仪器设备有限公司）。
1.3　方法
1.3.1　标准溶液的配制
准确吸取1.00 ml对羟基苯甲酸酯混合标准溶液，用乙腈稀释并定容至10 ml配制成质量浓度为100 μg/ml的混合标准中间溶液；准确吸取2.50 ml混合标准中间溶液，用乙腈稀释并定容至25 ml配制成质量浓度为10.0 μg/ml的混合标准工作溶液。准确吸取1.00 ml D4-对羟基苯甲酸乙酯标准溶液，用乙腈稀释并定容至10 ml配制成质量浓度为100 μg/ml的内标工作溶液。临用前，准确吸取适当体积的10.0 μg/ml的混合标准工作溶液于7支10 ml容量瓶中，分别加入0.10 ml内标工作溶液，用乙腈定容至刻度，摇匀，配制成内标物质量浓度均为1.00 μg/ml、各目标物质量浓度为0.05、0.10、0.25、0.50、1.00、2.50和5.00 μg/ml的标准系列工作溶液。
1.3.2　样品前处理
准确称取2.00 g均质化样品于50 ml离心管中，加入5 ml水，准确加入0.10 ml内标工作溶液和10 ml乙腈，然后加入一颗陶瓷均质子和ProElut QuE En萃取盐包中的试剂，立即以3 000 r/min涡旋振荡5 min，然后在0℃下16 093 ×g离心5 min；取6 ml上清液，加入ProElut QuE 15 ml净化管中，以3 000 r/min涡旋振荡2 min，静置后吸取上层液体过0.22 μm尼龙66膜过滤器，供GC-MS测试。
1.3.3　空白试验
除不加样品外，采用与试样操作完全相同的步骤进行。
1.3.4　分析条件
选用Agilent DB-5 MS UI毛细管色谱柱（规格30 m × 0.25 mm，0.25 μm）；程序升温：初始温度设定为70℃，保持2 min 后，以20℃/min的速率升至300℃，并保持2 min；进样口温度为280℃；进样方式为分流进样，分流比为1∶5；进样体积为1 μl；载气为高纯He，流量控制在1.0 ml/min。质谱离子源为电子轰击（EI）源，温度为300℃，电离能量为70eV；四极杆和传输线温度分别为150℃和280℃；溶剂延迟时间为5 min；检测模式为SIM。七种对羟基苯甲酸酯类化合物定量离子和定性离子等信息见表1。
1.3.5　结果计算
样品中对羟基苯甲酸酯类化合物含量按式（1）计算：
式中：Xi为样品中对羟基苯甲酸酯i的含量，mg/kg；c为由标准曲线计算得到样品测试液中对羟基苯甲酸酯i的质量浓度，μg/ml；c0为由标准曲线计算得到空白测试液中对羟基苯甲酸酯i的质量浓度，μg/ml；V为试样提取液体积，ml；m为取样量，g；1 000为单位换算系数。
2　结果
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2.1　提取溶剂的选择
对羟基苯甲酸酯类化合物具极性和非极性结构，其在水中溶解度较低，而在甲醇、乙醚、乙腈等有机溶剂中具有较高溶解度。乙醚与甲醇常被用作该类防腐剂的提取溶剂[13,20,26]，但牛油火锅底料富含甘油三酯等非极性脂类成分及色素等杂质易与甲醇、乙醚发生共萃取，导致提取体系中杂质含量偏高。乙腈与脂类物质的互溶性较低，可减少脂类杂质的共萃取，乙腈与水混合后，在盐析作用下快速分层，而脂类更易留在两相界面，进一步减少进入乙腈相的机会。因此，本研究选用乙腈作为对羟基苯甲酸酯类防腐剂的提取溶剂。
2.2　QuEChERS提取、净化
随着QuEChERS技术的日益成熟，市场上已涌现多种标准化的萃取盐包及净化管产品，为复杂基质样品（如高脂食品）的前处理提供了便捷的解决方案。本研究采用商业化QuEChERS试剂盒对牛油火锅底料样品进行提取和净化处理。样品加入适量水和提取溶剂后，加入ProElut QuE EN萃取盐包后立即高速涡旋振荡提取。MgSO4可快速吸收水分、放热融化并破坏油脂层，促进乙腈对目标物的萃取；NaCl可提高水相离子强度，加速乙腈-水两相的分层进程，促进目标物向乙腈相转移；柠檬酸钠/柠檬酸氢二钠缓冲体系维持弱酸性环境，不仅可抑制目标物的水解反应，还能降低基质中酸性干扰物质的共萃取。涡旋振荡处理后，通过低温离心操作促使牛油基质中的脂类成分发生冷凝团聚与沉降，从而进一步降低提取液中脂肪类杂质残留量。
考虑到牛油火锅底料基质中有机酸、色素、脂肪酸等杂质可能会对目标物的分析测定产生干扰，采用成品ProElut QuE 15 ml净化管对乙腈提取液进行净化处理。PSA通过氢键、离子交换等作用选择性吸附极性杂质；C18通过疏水相互作用选择性吸附样品中的脂肪、脂溶性色素等非极性基质成分；Carb对辣椒红素等具有平面结构的色素具有较强的吸附能力；MgSO4可快速去除提取液中残留的痕量水分。这些试剂协同作用，能够减少提取液中的杂质含量，降低其对目标物信号的干扰。净化处理后，提取液颜色明显变淡，干扰显著降低。
2.3　基质效应
对于牛油火锅底料这类基质组成复杂的样品，基质效应（matrix effect,ME）是必须考虑的影响因素。用纯溶剂和空白基质溶液配制质量浓度为1.00 μg/ml的对羟基苯甲酸酯混合标准溶液，分别测定目标物的信号响应值，并依据公式ME（%）=（空白基质标准溶液响应值/纯溶剂标准溶液响应值）×100评价基质效应。ME>100%和ME<100%分别提示存在基质增强和基质抑制效应，且ME值与100%偏差越大表明基质效应越强。结果显示七种对羟基苯甲酸酯类化合物的ME值均大于300%，说明牛油火锅底料对对羟基苯甲酸酯类防腐剂的测定呈现明显的基质增强效应。采用同位素内标进行校正是减少基质效应影响的重要手段。本研究选取D4-对羟基苯甲酸乙酯作为内标物，分别采用纯溶剂和空白基质溶液配制相同质量浓度（1.00 μg/ml）的标准溶液（其中内标物的质量浓度均为1.00 μg/ml），通过对比两种溶液中目标物和内标物响应的比值，结果发现二者的百分比介于92%和105%之间，因此采用内标法可以充分抵消基质效应的影响，从而实现目标物的准确定量。
2.4　GS-MS条件的优化
本实验涉及的七种对羟基苯甲酸酯类防腐剂中，异丙酯与丙酯、异丁酯与丁酯互为同分异构体，其监测离子完全一致，因此需通过优化色谱条件实现分离以保证准确定性。文献报道显示，HP-5 MS [16]和OV-1701 MS [27]色谱柱可用于此类防腐剂的分离。本研究选用DB-5 MS UI毛细管色谱柱（30 m×0.25 mm，0.25 μm）对待测目标物进行分离。实验过程中，通过全扫描模式在50～400 amu范围内筛选各目标物的特征离子，并对进样口温度、色谱柱升温程序、进样模式、分流比、离子源温度及传输线温度等关键仪器参数进行了优化，最终确定了分析条件。优化后的方法可在15 min内完成所有目标物的基线分离，且信号强度满足定量要求。在此条件下，混合标准溶液（1.00 μg/ml）及空白样品加标（5.00 mg/kg）处理后测试液的的总离子谱图见图1。
2.5　方法学考察
2.5.1　线性范围、检出限和定量限
在本法线性范围内，回归方程的相关系数（r）均大于0.999。取空白牛油火锅底料基质进行加标回收试验，以S/N=3和S/N=10所对应的加标水平分别估算方法的检出限和定量限。方法的回归方程、检出限和定量限评估结果见表2。
2.5.2　准确度和精密度
准确称取2.00 g空白样品，分别加入不同体积100 μg/ml或10.0 μg/ml混合标准溶液配制成高、中、低三个加标水平，每个水平平行制备6份，按本法处理后进样分析。回收率和精密度测定结果见表3。七种目标物在不同加标水平的平均回收率为91.4%～108%，相对标准偏差为0.6%～7.2%（n=6），表明该方法具有较好的准确度和精密度。
2.6　实际样品的测定
从自本地超市和干杂店采购不同品牌牛油火锅底料十份，按本法进行处理后测定七种对羟基苯甲酸酯类防腐剂的含量。其中二份样品检出对羟基苯甲酸甲酯，含量分别为10.5和6.25 mg/kg；一份样品同时检出对羟基苯甲酸甲酯和对羟基苯甲酸乙酯，含量分别为7.40和5.11 mg/kg。检测结果均符合《食品安全国家标准食品添加剂使用标准》（GB 2760—2024）中0.25 g/kg（以对羟基苯甲酸计）的限量规定[11]。
3　结论
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本研究建立了QuEChERS前处理结合GC-MS同时测定牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的方法。该方法操作简单、提取效率高、净化效果好、灵敏度、准确度和精密度高，能够满足牛油火锅底料中七种对羟基苯甲酸酯类防腐剂的检测要求。基于牛油火锅底料高盐、高脂的特点，本研究所建方法的适用范围或可扩展至其它类型预制食品（如各种复合调味料、预制菜、方便面等）；对环境基质和化妆品等其它类型的样品，采用本研究所建方法时需要开展基质效应分析、方法验证以确保其适用性。

文献
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2026年第53卷第1期
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doi: 10.20043/j.cnki.MPM.202508373
  • 接收时间：2025-08-23
  • 首发时间：2026-11-02
  • 出版时间：2026-01-10
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  • 收稿日期：2025-08-23
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    1.四川省疾病预防控制中心，四川 成都 610041
    2.达州市疾病预防控制中心

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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
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