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Article(id=1322589987506336096, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1322589954702688372, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202405310, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1715961600000, receivedDateStr=2024-05-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1793259625554, onlineDateStr=2026-10-29, pubDate=1736438400000, pubDateStr=2025-01-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793259625554, onlineIssueDateStr=2026-10-29, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793259625554, creator=13701087609, updateTime=1793259625554, updator=13701087609, issue=Issue{id=1322589954702688372, tenantId=1146029695717560320, journalId=1227665162245664772, year='2025', volume='52', issue='1', pageStart='1', pageEnd='192', issueExtLink='null', onlineDate='null', pubDate='1736438400000', pubDateStr='2025-01-10', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793259617734, creator='13701087609', updateTime=1793260023378, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322591656147276425, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1322589954702688372, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322591656147276426, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1322589954702688372, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=149, endPage=154, ext={EN=ArticleExt(id=1322589988005458273, articleId=1322589987506336096, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Solid phase extraction-gas chromatography-tandem mass spectrometry method for determining 21 types of herbicides in drinking water, columnId=1228016572065837304, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish a gas chromatography-tandem mass spectrometry (GC-MS/MS) method for detecting 21 types of herbicides in drinking water based on solid phase extraction (SPE) pre-treatment technology.

Methods

A 500 ml water sample was extracted using a C18 solid phase extraction column, followed by elution with a 5 ml mixture of ethyl acetate and dichloromethane (1:1). The eluent was collected and concentrated near dryness using vacuum centrifugation, and then reconstituted with 1 ml of ethyl acetate for analysis by gas chromatography-mass spectrometry in multiple reaction monitoring (MRM) mode.

Results

Within the concentration range of 5.0 μg/L to 200.0 μg/L, the herbicides exhibited good linearity, with correlation coefficients ranging from 0.9 954 to 0.9 998. The limits of detection (LOD) ranged from 0.11 μg/L to 1.21 μg/L, while the limits of quantification (LOQ) ranged from 0.33 μg/L to 3.64 μg/L. Precision (RSD) was found to be between 1.6% and 6.3%, and the recovery rates ranged from 74.3% to 112.7%.

Conclusion

This method demonstrates a wide linear range, accuracy, and reliability, making it suitable for the detection of multiple herbicides in water.

, authors=Yu DING, Rui ZHOU, Bo ZHANG, Li-li SONG, authorsList=Yu DING, Rui ZHOU, Bo ZHANG, Li-li SONG, authorCompany=null, correspAuthors=Li-li SONG, 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=1322589989154697572, articleId=1322589987506336096, tenantId=1146029695717560320, journalId=1227665162245664772, language=CN, title=固相萃取-气相色谱-串联质谱法测定生活饮用水中21种除草剂, 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

基于固相萃取前处理技术，建立生活饮用水中21种除草剂的气相色谱-串联质谱检测方法。

方法

抽取500 ml水样，经C18固相萃取小柱萃取、5 ml乙酸乙酯-二氯甲烷（1∶1）混合液洗脱。收集洗脱液，真空离心浓缩至近干，用1 ml乙酸乙酯定容后，进样气相色谱质谱仪检测、多反应监测模式（MRM）定量。

结果

在5.0～200.0 μg/L范围内，各除草剂呈现良好的线性，相关系数在0.995 4～0.999 8之间，检出限（LOD）在0.11～1.21 μg/L之间，定量限（LOQ）在0.33～3.64 μg/L之间，精密度（RSD）在1.6%～6.3%范围内，回收率在74.3%～112.7%之间。

结论

该方法线性范围宽、准确、可靠，适合于水中多种除草剂的检测。

, authors=丁宇, 周睿, 张博, 宋黎黎, authorsList=丁宇, 周睿, 张博, 宋黎黎, authorCompany=null, correspAuthors=宋黎黎, authorNote=

丁宇（1978—），男，本科，副主任技师，研究方向：理化检测工作

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宋黎黎，E-mail:
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GB 5009.295-2023 National food safety standards general rules for validation of chemical analysis methods[S].Beijing: Standards Press of China.(In Chinese), articleTitle=null, refAbstract=null)], funds=[Fund(id=1322590004702982547, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, awardId=2023PYZK04, language=CN, fundingSource=上海市黄浦区医学优势专科(2023PYZK04), fundOrder=null, country=null), Fund(id=1322590004786868628, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, awardId=HLM202224, language=CN, fundingSource=上海市黄浦区科学委员会课题(HLM202224), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1322589989662208357, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, xref=null, ext=[AuthorCompanyExt(id=1322589989670596966, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, companyId=1322589989662208357, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Shanghai Huangpu District Center for Disease Prevention and Control, Shanghai 200023, China), AuthorCompanyExt(id=1322589989674791271, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, companyId=1322589989662208357, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市黄浦区疾病预防控制中心，上海 200023)])], figs=[ArticleFig(id=1322589999241998727, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Figure 1, caption=The total ion flux (MRM) of 21 herbicides, figureFileSmall=GtQTb9ho+qyPNJXVOr/VgA==, figureFileBig=5MnRbH0r5M+f+S0oHF5HZA==, tableContent=null), ArticleFig(id=1322589999636263304, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=图1, caption=21种除草剂总离子流图（MRM）

注：1-硫草敌、2-敌草腈、3-禾草敌、4-环草敌、5-氟草胺、6-异噁草酮、7-去草净、8-炔苯酰草胺、9-敌草净、10-乙草胺、11-嗪草酮、12-扑草净、13-异丙甲草胺、14-禾草丹、15-氟丁酰草胺、16-丁草胺、17-抑草磷、18-敌草胺、19-丙草胺、20-噁草酮、21-除草醚。

, figureFileSmall=GtQTb9ho+qyPNJXVOr/VgA==, figureFileBig=5MnRbH0r5M+f+S0oHF5HZA==, tableContent=null), ArticleFig(id=1322590000462541193, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Table 1, caption=

The retention time, qualitative ions, quantitative ions, and collision energy of 21 herbicides

, figureFileSmall=null, figureFileBig=null, tableContent=
除草剂保留时间（min）定量离子（m/z）定性离子（m/z）
母离子子离子碰撞能量（ev）母离子子离子碰撞能量（ev）
硫草敌4.408100.0072.105.00161.00100.105.00
敌草腈6.260171.00136.0015.00171.00100.1025.00
禾草敌9.283126.0055.1015.0083.0055.105.00
环草敌10.94883.0055.1010.00154.0083.1010.00
氟草胺11.567292.00159.9030.00292.00264.105.00
异噁草酮13.337125.0089.0025.00204.00107.0020.00
去草净13.502169.00154.1010.00169.0069.1030.00
炔苯酰草胺13.892173.00144.9020.00175.00146.9015.00
敌草净15.618198.00108.0010.00198.0057.2030.00
乙草胺15.626213.00125.3015.00162.00147.1015.00
嗪草酮15.935198.0082.1015.00198.0055.1035.00
扑草净16.402241.0058.1010.00226.00184.0010.00
异丙甲草胺17.328238.00162.1010.00162.00133.0015.00
禾草丹17.421100.0072.105.00125.0089.1015.00
氟丁酰草胺19.312176.0091.1010.0091.0065.1020.00
丁草胺20.051188.00160.1015.00160.00130.1030.00
抑草磷20.413286.00185.0025.00286.00202.2015.00
敌草胺20.578128.0072.105.00271.00128.105.00
丙草胺20.813162.00147.1010.00162.00132.1020.00
噁草酮21.092175.00112.0015.00258.00175.0010.00
除草醚22.079128.0072.105.00271.00128.105.00
), ArticleFig(id=1322590000550621578, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=表1, caption=

21种除草剂的保留时间、定性离子、定量离子和碰撞能量

, figureFileSmall=null, figureFileBig=null, tableContent=
除草剂保留时间（min）定量离子（m/z）定性离子（m/z）
母离子子离子碰撞能量（ev）母离子子离子碰撞能量（ev）
硫草敌4.408100.0072.105.00161.00100.105.00
敌草腈6.260171.00136.0015.00171.00100.1025.00
禾草敌9.283126.0055.1015.0083.0055.105.00
环草敌10.94883.0055.1010.00154.0083.1010.00
氟草胺11.567292.00159.9030.00292.00264.105.00
异噁草酮13.337125.0089.0025.00204.00107.0020.00
去草净13.502169.00154.1010.00169.0069.1030.00
炔苯酰草胺13.892173.00144.9020.00175.00146.9015.00
敌草净15.618198.00108.0010.00198.0057.2030.00
乙草胺15.626213.00125.3015.00162.00147.1015.00
嗪草酮15.935198.0082.1015.00198.0055.1035.00
扑草净16.402241.0058.1010.00226.00184.0010.00
异丙甲草胺17.328238.00162.1010.00162.00133.0015.00
禾草丹17.421100.0072.105.00125.0089.1015.00
氟丁酰草胺19.312176.0091.1010.0091.0065.1020.00
丁草胺20.051188.00160.1015.00160.00130.1030.00
抑草磷20.413286.00185.0025.00286.00202.2015.00
敌草胺20.578128.0072.105.00271.00128.105.00
丙草胺20.813162.00147.1010.00162.00132.1020.00
噁草酮21.092175.00112.0015.00258.00175.0010.00
除草醚22.079128.0072.105.00271.00128.105.00
), ArticleFig(id=1322590000881971595, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Table 2, caption=

The recovery efficiency of each small column extraction

, figureFileSmall=null, figureFileBig=null, tableContent=
固相萃取小柱C18HLBC-NH2
回收率（%）74.3～112.765.3～90.740.8～76.2
), ArticleFig(id=1322590001360122252, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=表2, caption=

各小柱萃取的回收效果

, figureFileSmall=null, figureFileBig=null, tableContent=
固相萃取小柱C18HLBC-NH2
回收率（%）74.3～112.765.3～90.740.8～76.2
), ArticleFig(id=1322590001729221005, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Table 3, caption=

The optimization of eluent immersion time

, figureFileSmall=null, figureFileBig=null, tableContent=
静置时间（s）0306090
回收率（%）42.1～68.856.2～90.474.3～112.773.1～110.5
), ArticleFig(id=1322590001808912782, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=表3, caption=

洗脱剂浸没时间的优化

, figureFileSmall=null, figureFileBig=null, tableContent=
静置时间（s）0306090
回收率（%）42.1～68.856.2～90.474.3～112.773.1～110.5
), ArticleFig(id=1322590003809595791, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Table 4, caption=

The linear equations, correlation coefficients, detection limits, and quantification limits of 21 herbicides

, figureFileSmall=null, figureFileBig=null, tableContent=
除草剂线性方程相关系数LOD（μg/L）LQD（μg/L）
硫草敌y=2 541.9x+5 792.20.998 90.581.74
敌草腈y=2 446.2x-6 359.80.999 00.571.71
禾草敌y=2 447.61x-12 957.70.996 80.601.80
环草敌y=3 357.43x-16 885.90.996 50.712.12
氟草胺y=240.45x-1 464.90.997 11.123.35
异噁草酮y=670.54x-1 027.00.999 80.230.69
去草净y=195.82x+88.170.998 10.962.88
炔苯酰草胺y=376.41x-562.230.998 20.401.20
敌草净y=346.92x+87.480.999 21.213.64
乙草胺y=263.63x-236.550.999 80.952.85
嗪草酮y=105.55x+78.130.996 70.772.32
扑草净y=227.13x-946.460.996 91.073.20
异丙甲草胺y=1 212.22x-3 499.520.998 70.150.45
禾草丹y=2 152.93x-9 841.760.997 10.110.33
氟丁酰草胺y=356.44x-1 345.420.995 40.521.56
丁草胺y=49.05x-83.510.996 30.892.66
抑草磷y=70.51x-433.440.995 50.782.35
敌草胺y=377.77x-664.070.999 60.280.84
丙草胺y=388.73x-373.390.999 80.451.34
噁草酮y=895.45x-3 079.570.997 90.230.69
除草醚y=71.45x-410.440.996 10.732.18
), ArticleFig(id=1322590003906064784, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=表4, caption=

21种除草剂的线性方程、相关系数、检出限和定量限

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除草剂线性方程相关系数LOD（μg/L）LQD（μg/L）
硫草敌y=2 541.9x+5 792.20.998 90.581.74
敌草腈y=2 446.2x-6 359.80.999 00.571.71
禾草敌y=2 447.61x-12 957.70.996 80.601.80
环草敌y=3 357.43x-16 885.90.996 50.712.12
氟草胺y=240.45x-1 464.90.997 11.123.35
异噁草酮y=670.54x-1 027.00.999 80.230.69
去草净y=195.82x+88.170.998 10.962.88
炔苯酰草胺y=376.41x-562.230.998 20.401.20
敌草净y=346.92x+87.480.999 21.213.64
乙草胺y=263.63x-236.550.999 80.952.85
嗪草酮y=105.55x+78.130.996 70.772.32
扑草净y=227.13x-946.460.996 91.073.20
异丙甲草胺y=1 212.22x-3 499.520.998 70.150.45
禾草丹y=2 152.93x-9 841.760.997 10.110.33
氟丁酰草胺y=356.44x-1 345.420.995 40.521.56
丁草胺y=49.05x-83.510.996 30.892.66
抑草磷y=70.51x-433.440.995 50.782.35
敌草胺y=377.77x-664.070.999 60.280.84
丙草胺y=388.73x-373.390.999 80.451.34
噁草酮y=895.45x-3 079.570.997 90.230.69
除草醚y=71.45x-410.440.996 10.732.18
), ArticleFig(id=1322590004254192017, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=EN, label=Table 5, caption=

The spiked recovery and RSD of 21 herbicides

, figureFileSmall=null, figureFileBig=null, tableContent=
除草剂加标量(5.0 μg/L)加标量(25.0 μg/L)加标量(50.0 μg/L)
测定值(μg/L)回收率（%）RSD(%)测定值(μg/L)回收率（%）RSD(%)测定值(μg/L)回收率（%）RSD(%)
硫草敌4.181.25.721.284.74.543.286.33.6
敌草腈4.079.85.320.883.25.342.384.52.7
禾草敌5.3105.36.326.1104.54.755.1110.22.9
环草敌4.182.56.121.786.94.939.779.46.1
氟草胺4.385.46.222.690.33.743.286.45.8
异噁草酮4.386.34.223.794.71.945.290.35.3
去草净4.181.95.522.489.42.542.484.72.7
炔苯酰草胺3.774.35.719.678.52.938.075.93.5
敌草净3.978.65.820.983.63.638.777.33.7
乙草胺4.793.44.923.794.83.345.691.23.8
嗪草酮4.692.74.822.991.64.247.394.54.6
扑草净4.590.45.023.393.24.648.196.24.8
异丙甲草胺5.1101.86.124.296.94.151.9103.85.6
禾草丹5.6112.74.726.2104.72.955.2110.46.2
氟丁酰草胺5.2104.34.823.895.13.852.6105.15.1
丁草胺4.793.14.923.393.24.548.296.31.6
抑草磷4.488.45.322.489.73.646.392.62.4
敌草胺4.284.55.422.991.43.746.893.63.1
丙草胺3.978.65.421.284.74.641.382.53.8
噁草酮4.079.45.621.887.34.343.286.43.6
除草醚3.875.65.322.891.34.444.488.74.7
), ArticleFig(id=1322590004363243922, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1322589987506336096, language=CN, label=表5, caption=

21种除草剂的加标回收率及RSD

, figureFileSmall=null, figureFileBig=null, tableContent=
除草剂加标量(5.0 μg/L)加标量(25.0 μg/L)加标量(50.0 μg/L)
测定值(μg/L)回收率（%）RSD(%)测定值(μg/L)回收率（%）RSD(%)测定值(μg/L)回收率（%）RSD(%)
硫草敌4.181.25.721.284.74.543.286.33.6
敌草腈4.079.85.320.883.25.342.384.52.7
禾草敌5.3105.36.326.1104.54.755.1110.22.9
环草敌4.182.56.121.786.94.939.779.46.1
氟草胺4.385.46.222.690.33.743.286.45.8
异噁草酮4.386.34.223.794.71.945.290.35.3
去草净4.181.95.522.489.42.542.484.72.7
炔苯酰草胺3.774.35.719.678.52.938.075.93.5
敌草净3.978.65.820.983.63.638.777.33.7
乙草胺4.793.44.923.794.83.345.691.23.8
嗪草酮4.692.74.822.991.64.247.394.54.6
扑草净4.590.45.023.393.24.648.196.24.8
异丙甲草胺5.1101.86.124.296.94.151.9103.85.6
禾草丹5.6112.74.726.2104.72.955.2110.46.2
氟丁酰草胺5.2104.34.823.895.13.852.6105.15.1
丁草胺4.793.14.923.393.24.548.296.31.6
抑草磷4.488.45.322.489.73.646.392.62.4
敌草胺4.284.55.422.991.43.746.893.63.1
丙草胺3.978.65.421.284.74.641.382.53.8
噁草酮4.079.45.621.887.34.343.286.43.6
除草醚3.875.65.322.891.34.444.488.74.7
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固相萃取-气相色谱-串联质谱法测定生活饮用水中21种除草剂
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丁宇 , 周睿 , 张博 , 宋黎黎
现代预防医学 | 实验技术及其应用 2025,52(1): 149-154
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现代预防医学 |实验技术及其应用 2025 , 52 (1) : 149 -154
固相萃取-气相色谱-串联质谱法测定生活饮用水中21种除草剂
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丁宇（1978—），男，本科，副主任技师，研究方向：理化检测工作

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丁宇, 周睿, 张博, 宋黎黎
作者信息
  • 上海市黄浦区疾病预防控制中心，上海 200023
通讯作者:
宋黎黎，E-mail:
作者简介:

丁宇（1978—），男，本科，副主任技师，研究方向：理化检测工作

Solid phase extraction-gas chromatography-tandem mass spectrometry method for determining 21 types of herbicides in drinking water
Yu DING, Rui ZHOU, Bo ZHANG, Li-li SONG
Affiliations
  • Shanghai Huangpu District Center for Disease Prevention and Control, Shanghai 200023, China
出版时间: 2025-01-10 doi: 10.20043/j.cnki.MPM.202405310
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摘要
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目的

基于固相萃取前处理技术，建立生活饮用水中21种除草剂的气相色谱-串联质谱检测方法。

方法

抽取500 ml水样，经C18固相萃取小柱萃取、5 ml乙酸乙酯-二氯甲烷（1∶1）混合液洗脱。收集洗脱液，真空离心浓缩至近干，用1 ml乙酸乙酯定容后，进样气相色谱质谱仪检测、多反应监测模式（MRM）定量。

结果

在5.0～200.0 μg/L范围内，各除草剂呈现良好的线性，相关系数在0.995 4～0.999 8之间，检出限（LOD）在0.11～1.21 μg/L之间，定量限（LOQ）在0.33～3.64 μg/L之间，精密度（RSD）在1.6%～6.3%范围内，回收率在74.3%～112.7%之间。

结论

该方法线性范围宽、准确、可靠，适合于水中多种除草剂的检测。

固相萃取  /  气相色谱-串联质谱法  /  生活饮用水  /  除草剂
Objective

To establish a gas chromatography-tandem mass spectrometry (GC-MS/MS) method for detecting 21 types of herbicides in drinking water based on solid phase extraction (SPE) pre-treatment technology.

Methods

A 500 ml water sample was extracted using a C18 solid phase extraction column, followed by elution with a 5 ml mixture of ethyl acetate and dichloromethane (1:1). The eluent was collected and concentrated near dryness using vacuum centrifugation, and then reconstituted with 1 ml of ethyl acetate for analysis by gas chromatography-mass spectrometry in multiple reaction monitoring (MRM) mode.

Results

Within the concentration range of 5.0 μg/L to 200.0 μg/L, the herbicides exhibited good linearity, with correlation coefficients ranging from 0.9 954 to 0.9 998. The limits of detection (LOD) ranged from 0.11 μg/L to 1.21 μg/L, while the limits of quantification (LOQ) ranged from 0.33 μg/L to 3.64 μg/L. Precision (RSD) was found to be between 1.6% and 6.3%, and the recovery rates ranged from 74.3% to 112.7%.

Conclusion

This method demonstrates a wide linear range, accuracy, and reliability, making it suitable for the detection of multiple herbicides in water.

Solid phase extraction  /  Gas chromatography-tandem mass spectrometry  /  Drinking water  /  Herbicides
丁宇, 周睿, 张博, 宋黎黎. 固相萃取-气相色谱-串联质谱法测定生活饮用水中21种除草剂. 现代预防医学, 2025 , 52 (1) : 149 -154 . DOI: 10.20043/j.cnki.MPM.202405310
Yu DING, Rui ZHOU, Bo ZHANG, Li-li SONG. Solid phase extraction-gas chromatography-tandem mass spectrometry method for determining 21 types of herbicides in drinking water[J]. Modern Preventive Medicine, 2025 , 52 (1) : 149 -154 . DOI: 10.20043/j.cnki.MPM.202405310
正文
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为了提高粮食产量，减少杂草对农作物营养、水分和阳光的争夺，各类除草剂相继开发并广泛用于农业生产。目前，丙草胺和丁草胺等多用与水稻田杂草抑制,而其他除草剂则用于旱田除草[1-2]。除草剂喷洒在农田后，部分会残留在土壤和空气中。相对于土壤吸附，除草剂更易溶于水，并逐步渗透至地下水，造成水源污染，最终通过食物链进入人体，干扰激素平衡，损坏神经系统，造成智力低下、多动症、过敏性疾病等，甚至诱发癌症，严重危害人体健康和生命安全[3-5]。
目前常见的除草剂检测方法主要有胶体金免疫分析法[6]、气相色谱法[7-9]、液相色谱法[10]、气相色谱-质谱法[11-12]、液相色谱-质谱法[13]等。柯童炜等[6]采用试纸条上固定的抗体识别、捕获样品中的扑草净，通过颜色变化半定量检测扑草净残留。但该方法仅能对部分除草剂进行分析，不适于多种待测组分的同时检测，且定量能力相较其他分析方法略显不足。张妮娜等[9]建立了地表水中甲草胺和乙草胺的气相色谱法测定方法；吴亮等[10]利用高效液相色谱法检测了稻田样品中禾草灵等5种除草剂。但是气相色谱法和液相色谱法检测灵敏度不高，且定性能力有限，近年来逐渐被质谱法替代；石莹等[14]采用液相色谱-质谱法测定了稻田水体中丙草胺、丁草胺等8种常用除草剂残留，取得了较好的效果。
气相色谱-串联质谱法具有卓越的定性能力和高灵敏度等优点，能够满足多种除草剂准确、灵敏、可靠检测的需求。本文分析的21种除草剂，多为硫代氨基甲酸酯类、三嗪类和酰胺类除草剂，极性相对较弱，C18小柱对其具有良好的保留能力。鉴于此，本研究采用C18固相萃取小柱对目标待测物进行萃取和富集，再通过气相色谱-串联质谱法检测，此方法操作简便、准确可靠、结果满意。
1　材料与方法
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1.1　仪器与试剂
GCMS-TQ8040 NXNC气相色谱串联质谱仪（日本岛津公司）；EZ-2真空浓缩仪（英国Genevac公司）；VF-5MS色谱柱（30 m×0.25 mm，0.25 μm，美国瓦里安公司）；0.45 μm尼龙针头过滤器。氮气：纯度不小于99.999%；氦气：纯度不小于99.999%（上海优华气体有限公司）。
硫草敌、敌草腈、禾草敌、环草敌、氟草胺、异噁草酮、去草净、炔苯酰草胺、敌草净、乙草胺、嗪草酮、扑草净、异丙甲草胺、禾草丹、氟丁酰草胺、丁草胺、抑草磷、敌草胺、丙草胺、噁草酮和除草醚标准物质，浓度均为100 μg/ml（天津阿尔塔科技有限公司）。
乙酸乙酯（HPLC级，德国默克公司）；二氯甲烷（HPLC级，德国默克公司）；甲醇（HPLC级，德国默克公司）；CNW PolySery C18小柱（200 mg，6 ml）（上海安谱公司）。
1.2　方法
1.2.1　标准曲线的配制
1.2.1.1　混合标准中间液的配制
准确吸取0.5 ml各标准物质原液于50 ml容量瓶中，用乙酸乙酯定容，可得1 000 μg/L的混合标准中间液。
1.2.1.2　混合标准应用液的配制
分别取混合标准中间液50、100、200、500、1 000和2 000 μl，用乙酸乙酯定容至10 ml，配制成浓度为5.0、10.0、20.0、50.0、100.0和200.0 μg/L混合标准应用液。
1.2.2　样品制备
使用具有聚四氟乙烯瓶垫的2 L广口棕色玻璃瓶采集地下管网水样，取水至满瓶，加入0.2 g抗坏血酸，除去余氯，密封后送至实验室，4℃放置24 h。检测前用0.45 μm滤膜过滤水样。
1.2.3　固相萃取
1.2.3.1　C18小柱的活化　依次用5 ml二氯甲烷、5 ml乙酸乙酯过柱，真空泵抽干30 s，再依次用10 ml甲醇、10 ml纯水在重力作用下过柱活化，使用控流阀控制液面，保持吸附剂不暴露于空气中。
1.2.3.2　准确量取500 ml水样，以15 ml/min流速过C18小柱。抽干水分，在C18小柱上加入5 ml乙酸乙酯和二氯甲烷（1∶1）混合液，静置60 s后，在重力作用下洗脱，并收集洗脱液。将洗脱液置于真空浓缩仪中，浓缩至近干。用乙酸乙酯定容至1.0 ml，上机测定。
1.2.4　仪器条件
1.2.4.1　色谱条件
色谱柱：VF-5MS 30m×0.25 mm，0.25 μm；载气：氦气，流速为1.0 ml/min；进样口温度：280 ℃；升温程序：初始温度为60 ℃，保持1 min，先以40 ℃/min升至120 ℃，再以5 ℃/min升至310 ℃，保持4.5 min；进样量为1 μl。
1.2.4.2　质谱条件
离子源温度：230 ℃；接口温度：280 ℃；溶剂延迟时间：3 min；电离方式：电子轰击电离（EI）；电离能量：70 eV；扫描间隔：0.30 s；监测扫描模式：MRM模式；碰撞气：氩气。
2　结果
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2.1　色谱条件的优化
考察了VF-5MS 、VF-1701和VF-1MS三种不同填料（柱长、粒径和涂层厚度一致）的色谱柱的分离效果，使用VF-5MS时21种待测物可实现较好分离，峰形尖锐，且同一浓度的待测物相应信号较后两者略大；而使用后两种色谱柱时，部分除草剂色谱峰重叠，不能完全分离。故选择VF-5MS用于后续分离。同时，优化了升温程序，确保目标组分能得到良好的分离，峰形对称且尖锐。
2.2　质谱条件的优化
首先采用SCAN模式对21种除草剂进行扫描，确定各待测物的保留时间，选择相对丰度较高、干扰少的特征碎片峰作为母离子，通过仪器自带优化程序，辅以人工筛选，优选出最适合的碰撞能量以及二级碎片离子，再用MRM模式对子离子进行检测，最终确定21种目标组分的保留时间、定性离子、定量离子和碰撞能量见表1、图1。
2.3　固相萃取柱的选择
将加标0.1 μg/L的500 ml水样分别使用C18小柱、HLB小柱、C-NH2柱进行萃取，结果表明，水样经HLB小柱、C-NH2柱处理后，基线偏高，杂峰较多，萃取效果欠佳；而水样经C18小柱处理后，样品中杂质离子得到有效去除，基线稳定，杂峰较少，待测物分离效果良好。各小柱萃取的回收效果见表2。
综上，C18小柱能有效去除样品中的基质干扰，回收效果也最为理想，故本文选用C18小柱用于固相萃取前处理。
2.4　洗脱剂的优化
分别使用5 ml乙酸乙酯、5ml二氯甲烷、5 ml乙酸乙酯-二氯甲烷（1∶1）、5 ml乙酸乙酯-二氯甲烷（2∶1）作为洗脱液，对加标0.1 μg/L的500 ml水样进行回收实验，回收率依次54.2%～79.0%、38.6%～64.9%、74.3%～112.7%、62.7%～87.4%。结果表明，采用乙酸乙酯-二氯甲烷（1∶1）洗脱时，各待测除草剂的回收效果更理想，故选择5 ml乙酸乙酯-二氯甲烷（1∶1）作为洗脱液。
2.5　洗脱剂浸没时间的选择
在控流阀关闭状态下，将洗脱剂加入C18小柱，待洗脱剂完全浸没填料层，并静置片刻，使吸附在填料上的除草剂充分置换到洗脱剂中。本文考察了浸没时长分别为0、30、60和90 s的回收率，结果见表3。
经比较发现，大部分除草剂随洗脱剂浸没时间延长，回收率逐步升高，至60 s时可达到74.3%～112.7%，而浸没90与60 s的回收率无明显差异，故选择60 s作为洗脱剂浸没时长。
2.6　标准曲线方程及检出限
在5.0～200.0 μg/L范围内，以待测物的浓度为横坐标，待测物的响应值为纵坐标，绘制标准曲线，所有待测组分均呈现良好的线性关系。配制1.0 μg/L除草剂混合标准溶液，连续测定6次，以3倍信噪比计算检出限（LOD）、10倍信噪比计算定量限（LQD）[15]。结果见表4。
21种除草剂的检出限（LOD）在0.11～1.21 μg/L之间，定量限（LOQ）在0.33～3.64 μg/L范围内。
2.7　加标回收及精密度试验
以纯水作为空白水样，对其进行高、中、低浓度的加标试验，并分别连续测定6次，测定回收率和RSD，结果见表5。
由表5可知，21种除草剂回收率为74.3 %～112.7%，RSD为1.6 %～6.3 %，表明所建立的方法准确且可靠。
2.8　实际样品分析
采用本方法对30件生活饮用水样品进行检测，1件样品检出乙草胺，浓度为0.018 μg/L，其余水样均未检出所测的除草剂成分。
3　讨论
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进入水体的除草剂，浓度较低，通常需要进行提取和浓缩处理。固相萃取技术基于液固色谱萃取原理，利用除草剂和杂质组分在吸附剂上分配、吸附和离子交换能力的差异，将待测组分与杂质分离，从而降低样品基体干扰、提高检测的灵敏度和准确度。
C18固相萃取小柱是基于十八烷基键合硅胶的反相萃取介质，它对非极性到弱极性的有机化合物具有较好的保留能力，而本研究分析的21种除草剂极性均较弱，因此C18柱能够有效地富集和纯化这些目标分析物。另外，C18柱与水、含水缓冲液和大多数有机溶剂兼容性好，因此可灵活选择样品处理条件。
乙酸乙酯和二氯甲烷的极性各不相同，但是将其以1∶1混合后作为洗脱剂，则可以改变溶剂的极性，从而获得比单一试剂更广泛的极性选择范围，从而改善对部分除草剂的洗脱效果。加入洗脱剂后，需要浸没60 s左右，以便让吸附在SPE小柱填料中的除草剂被充分洗脱并转移至洗脱剂中，从而提高检出率。但是浸没时间不可过长，因为二氯甲烷易挥发，暴露在空气中时间过长会由于挥发而影响测定结果。
VF-5MS是一种高惰性的5%苯基甲基聚硅氧烷色谱柱，比VF-1MS固定相极性稍高，而较VF-1701极性弱，适于兼顾对非极性除草剂和弱极性除草剂的分离，具有更高的检测灵敏度和分离效果。
综上，本文建立了生活饮用水中21种除草剂的固相萃取-气相色谱-串联质谱法测定方法，所建立的方法灵敏、准确、可靠，适于推广应用。
基金
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  • 上海市黄浦区医学优势专科(2023PYZK04)
  • 上海市黄浦区科学委员会课题(HLM202224)
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doi: 10.20043/j.cnki.MPM.202405310
  • 接收时间：2024-05-18
  • 首发时间：2026-10-29
  • 出版时间：2025-01-10
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  • 收稿日期：2024-05-18
基金
上海市黄浦区医学优势专科(2023PYZK04)
上海市黄浦区科学委员会课题(HLM202224)
作者信息
    上海市黄浦区疾病预防控制中心，上海 200023

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2种不同金属材料的力学参数
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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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