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Article(id=1241522856148923206, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241522846384583426, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202308392, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1692460800000, receivedDateStr=2023-08-20, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773931715284, onlineDateStr=2026-03-19, pubDate=1707494400000, pubDateStr=2024-02-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773931715284, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773931715284, creator=13701087609, updateTime=1773931715284, updator=13701087609, issue=Issue{id=1241522846384583426, tenantId=1146029695717560320, journalId=1227665162245664772, year='2024', volume='51', issue='3', pageStart='385', pageEnd='576', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773931712956, creator=13701087609, updateTime=1773931842201, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241523388544504301, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241522846384583426, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241523388544504302, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241522846384583426, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=523, endPage=528, ext={EN=ArticleExt(id=1241522856522216272, articleId=1241522856148923206, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Determination of 33 organophosphorus pesticide residues in different fruit and vegetable substrates by QuEChERs combined with gas chromatography-tandem mass spectrometry, columnId=1228016572065837304, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish a rapid method for the determination of 33 organophosphorus pesticide residues in four different fruit and vegetable substrates (common type, high pigment type, high fat type, and high sugar type) by QuEChERs pretreatment combined with gas chromatography-tandem mass spectrometry (GC-MS), so as to provide technical support for simultaneous detection and food safety risk assessment of organophosphorus pesticides in different fruits and vegetables.

Methods

The samples were extracted with acetonitrile and sodium citrate-disodium hydrogen citrate buffer at the same time, purified with ethylenediamine-N-propyl silane (PSA), octadecylsilane bonded silica gel (C18), and graphitized carbon black (GCB). After nitrogen blowing concentration, the samples were re-dissolved with acetone and detected by gas chromatography-tandem mass spectrometry under multi-reaction ion monitoring (MRM) mode. Quantifications were based on internal standard curves.

Results

The method had good linear relationship in the range of 50 μg/L to 500 μg/L, with the correlation coefficients greater than 0.9950. The detection limits were within 1.50 to 5.04 μg/kg, and the limits of quantification were within 5.01 to 16.78 μg/kg. In the range of 0.040 to 0.200 mg/kg, the average recoveries ranged from 71.4% to 119.1%, with the relative standard deviations less than 12%.

Conclusion

The method is simple and rapid, with high accuracy and precision, which is suitable for the rapid detection and quantitative analysis of 33 organophosphorus pesticide residues in different fruit and vegetable substrates.

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目的

采用QuEChERs前处理结合气相色谱-串联质谱技术，建立四种不同果蔬基质（普通型、高色素型、高脂肪型及高糖型）中33种有机磷类农药残留量快速检测方法，为不同水果、蔬菜中多种有机磷农药同时检测和食品安全风险评估提供技术支持。

方法

样品经乙腈及柠檬酸钠-柠檬酸氢二钠缓冲液同时提取，乙二胺-N-丙基硅烷（PSA）、十八烷基硅烷键合硅胶（C18）及石墨化炭黑（GCB）三种吸附剂净化，氮吹浓缩后用丙酮复溶，采用气相色谱-串联质谱仪在多反应离子监测(MRM)模式下进行检测，内标法定量。

结果

四种不同果蔬基质中33种有机磷类农药在50～500 μg/L的浓度范围内相关系数均大于0.995 0，方法检出限为1.50～5.04 μg/kg，定量限为5.01～16.78 μg/kg；在添加0.040～0.200 mg/kg水平范围内，农药的平均回收率为71.4%～119.1%，相对标准偏差均低于12%。

结论

该方法简单快速、准确度高、精密度好，适用于不同果蔬基质中33种有机磷类农药残留的快速检测和定量分析。

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夏仕青，E-mail：
, copyrightStatement=本刊刊出的所有文章不代表中华预防医学会和本刊编委会的观点，除非特别声明。, copyrightOwner=中华预防医学会和四川大学华西公共卫生学院, extLink=null, articleAbsUrl=null, sourceXml=wqairBvT3dTykY34SLMzLg==, magXml=bdfA/uWI/jhqVdT6kjzgaA==, pdfUrl=null, pdf=XmQaiM4Xai0bCUae7PSIbA==, pdfFileSize=909293, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=g5cjpZ/AmzIgCM2vqGfP4A==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=bOZBB0A4Snu8rrYEHOPzDQ==, mapNumber=null, authorCompany=null, fund=null, authors=

夏仕青（1990—），女，硕士，主管技师及公卫医师，研究方向：环境及食品卫生检测

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夏仕青（1990—），女，硕士，主管技师及公卫医师，研究方向：环境及食品卫生检测

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Journal of Food Safety & Quality, 2020, 11(23): 8784-8792., articleTitle=Matrix effects analysis and determination method selection of organophosphrous pesticides in vegetables and fruits, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1241680449668444568, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, xref=null, ext=[AuthorCompanyExt(id=1241680449676833177, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, companyId=1241680449668444568, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Surveillance, Center for Disease Control and Prevention, Qianxinan Prefecture, Guizhou Province, Xingyi, Guizhou 562400, China), AuthorCompanyExt(id=1241680449685221786, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, companyId=1241680449668444568, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=贵州省黔西南州疾病预防控制中心监测检验科，贵州 兴义 562400)])], figs=[ArticleFig(id=1241680453770474103, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=EN, label=Figure 1, caption=MRM total ion flow chromatogram of the mixed solution of 33 organophosphorus pesticides and internal standard (5 mg/L), figureFileSmall=j2aWy62gqaCmGbqkLjjBMw==, figureFileBig=AvOphQpdXF9G2y5NNdd5VQ==, tableContent=null), ArticleFig(id=1241680453883720318, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=CN, label=图1, caption=33种有机磷农药及内标混合标准溶液（5 mg/L）的MRM总离子流色谱图, figureFileSmall=j2aWy62gqaCmGbqkLjjBMw==, figureFileBig=AvOphQpdXF9G2y5NNdd5VQ==, tableContent=null), ArticleFig(id=1241680454017938063, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=EN, label=Figure 2, caption=Recovery rates of different extraction methods in different substrates, figureFileSmall=wcWb6C9vK9hqdbIiuvdJ6A==, figureFileBig=upqmBBrCPXPvyBop754+uQ==, tableContent=null), ArticleFig(id=1241680454160544411, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=CN, label=图2, caption=不同提取方法和基质的加标回收率, figureFileSmall=wcWb6C9vK9hqdbIiuvdJ6A==, figureFileBig=upqmBBrCPXPvyBop754+uQ==, tableContent=null), ArticleFig(id=1241680454252819105, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=EN, label=Figure 3, caption=Recovery rates of different purification methods, figureFileSmall=y4Qzbpm7PUsgVrDZlXNfTA==, figureFileBig=JltO1o8+jfxXrrFNKvArkw==, tableContent=null), ArticleFig(id=1241680454378648235, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=CN, label=图3, caption=不同净化方法的回收率, figureFileSmall=y4Qzbpm7PUsgVrDZlXNfTA==, figureFileBig=JltO1o8+jfxXrrFNKvArkw==, tableContent=null), ArticleFig(id=1241680454462534320, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=EN, label=Table 1, caption=

Mass spectrometric parameters of the method

, figureFileSmall=null, figureFileBig=null, tableContent=
农药编号农药名称保留时间(min)离子对(m/z)碰撞电压(V)
1乙酰甲胺磷(Acephate)9.71136/42.1*，94/648，8
2莎稗磷(Anilofos)24.08225.9/157*，183.7/15714，8
3乙基谷硫磷(Azinphos-ethyl)25.51160/77*，132/5116，26
4溴苯烯磷(Bromfenvinphos)18.71323.1/266.9*，266.9/15910，14
5乙基溴硫磷(Bromophos-ethyl)18.06358.7/302.8*，96.9/6515，16
6溴硫磷(Bromophos)16.75330.8/315.8*，125/7914，6
7虫螨磷(Chlorthiophos)20.31324.9/269*，268.9/20512，14
8蝇毒磷(Coumaphos)27.11361.9/109*，209.9/11915，22
9百治磷(Dicrotophos)12.08192.7/127*，127/94.98，16
10敌瘟磷(Edifenphos)21.46310/109*，172.9/65.126，30
11灭线磷(Ethoprophos)11.71200/158*，157.9/96.96，16
12丰索磷(Fensulfothion)20.26307.9/96.9*，292/10926，15
13倍硫磷砜(Fenthion sulfone)20.46309.9/105*，135.9/9210，10
14倍硫磷亚砜(Fenthion sulfoxide)20.29278/109*，109/7915，8
15噻唑磷(Fosthiazate peak 1)16.73194.9/59.9*，194.9/102.916，8
16异稻瘟净(Iprobenfos)14.15203.9/91.1*，91.1/658，16
17异柳磷(Isofenphos)17.44213/121*，185/12114，10
18氧异柳磷(Isofenfos oxon)16.38228.9/121.1*，200.8/121.124，16
19马拉氧磷(Malaoxon)14.80127/55*，99/715，8
20虫螨畏(Methacrifos)10.43240/180*，125/7910，8
21速灭磷(Mevinphos)9.86192/127*，127/9510，14
22对氧磷(Paraoxon-ethyl)15.15149/91.1*，109/8110，10
23硫环磷(Phosfolan)17.34195.8/139.9*，139.9/6010，15
24磷胺(Phosphamidon)14.59264.1/127*，127/94.912，16
25哌草磷(Piperophos)23.60320.1/122.1*，122.1/5310，20
26嘧啶磷(Pirimiphos-ethyl)16.83318.1/166.1*，304/168.112，12
27哒嗪硫磷(Pyridaphenthion)23.20340/199.1*，199/77.18，24
28喹硫磷(Quinalphos)17.54157.1/102*，146/9122，30
29治螟磷(Sulfotep)12.21322/202*，202/145.910，10
30丁基嘧啶磷(Tebupirimfos)14.08261/137.1*，233.8/110.115，10
31特丁硫磷砜(Terbufos sulfone)17.21199/97*，125/9720，6
32甲基立枯磷(Tolclofos-methyl)14.17266.8/252*，265/9312，25
33脱叶磷(Tolclofos-methyl)18.29202/112.9*，169.3/57.116，6
34环氧七氯(Heptachlor epoxide B)17.00354.8/264.9*，352.8/262.912，16
), ArticleFig(id=1241680454546420409, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=CN, label=表1, caption=

方法的质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
农药编号农药名称保留时间(min)离子对(m/z)碰撞电压(V)
1乙酰甲胺磷(Acephate)9.71136/42.1*，94/648，8
2莎稗磷(Anilofos)24.08225.9/157*，183.7/15714，8
3乙基谷硫磷(Azinphos-ethyl)25.51160/77*，132/5116，26
4溴苯烯磷(Bromfenvinphos)18.71323.1/266.9*，266.9/15910，14
5乙基溴硫磷(Bromophos-ethyl)18.06358.7/302.8*，96.9/6515，16
6溴硫磷(Bromophos)16.75330.8/315.8*，125/7914，6
7虫螨磷(Chlorthiophos)20.31324.9/269*，268.9/20512，14
8蝇毒磷(Coumaphos)27.11361.9/109*，209.9/11915，22
9百治磷(Dicrotophos)12.08192.7/127*，127/94.98，16
10敌瘟磷(Edifenphos)21.46310/109*，172.9/65.126，30
11灭线磷(Ethoprophos)11.71200/158*，157.9/96.96，16
12丰索磷(Fensulfothion)20.26307.9/96.9*，292/10926，15
13倍硫磷砜(Fenthion sulfone)20.46309.9/105*，135.9/9210，10
14倍硫磷亚砜(Fenthion sulfoxide)20.29278/109*，109/7915，8
15噻唑磷(Fosthiazate peak 1)16.73194.9/59.9*，194.9/102.916，8
16异稻瘟净(Iprobenfos)14.15203.9/91.1*，91.1/658，16
17异柳磷(Isofenphos)17.44213/121*，185/12114，10
18氧异柳磷(Isofenfos oxon)16.38228.9/121.1*，200.8/121.124，16
19马拉氧磷(Malaoxon)14.80127/55*，99/715，8
20虫螨畏(Methacrifos)10.43240/180*，125/7910，8
21速灭磷(Mevinphos)9.86192/127*，127/9510，14
22对氧磷(Paraoxon-ethyl)15.15149/91.1*，109/8110，10
23硫环磷(Phosfolan)17.34195.8/139.9*，139.9/6010，15
24磷胺(Phosphamidon)14.59264.1/127*，127/94.912，16
25哌草磷(Piperophos)23.60320.1/122.1*，122.1/5310，20
26嘧啶磷(Pirimiphos-ethyl)16.83318.1/166.1*，304/168.112，12
27哒嗪硫磷(Pyridaphenthion)23.20340/199.1*，199/77.18，24
28喹硫磷(Quinalphos)17.54157.1/102*，146/9122，30
29治螟磷(Sulfotep)12.21322/202*，202/145.910，10
30丁基嘧啶磷(Tebupirimfos)14.08261/137.1*，233.8/110.115，10
31特丁硫磷砜(Terbufos sulfone)17.21199/97*，125/9720，6
32甲基立枯磷(Tolclofos-methyl)14.17266.8/252*，265/9312，25
33脱叶磷(Tolclofos-methyl)18.29202/112.9*，169.3/57.116，6
34环氧七氯(Heptachlor epoxide B)17.00354.8/264.9*，352.8/262.912，16
), ArticleFig(id=1241680454647083714, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=EN, label=Table 2, caption=

Recovery rates and relative standard deviations (%) of different spiked levels in different substrates

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称加标1（0.040 mg/kg）加标2（0.125 mg/kg）加标3（0.200 mg/kg）
平均回收率相对标准偏差平均回收率相对标准偏差平均回收率相对标准偏差
苹果80.5～117.32.6～9.694.3～114.61.6～6.675.0～111.82.2～9.7
黄瓜81.9～118.33.3～10.281.1～107.94.1～9.872.8～108.61.2～6.4
香蕉76.0～118.03.0～8.177.7～109.93.6～7.974.5～116.13.1～9.4
土豆73.8～113.92.3～9.574.3～103.22.1～7.672.0～100.23.8～12.0
草莓82.5～118.01.9～9.289.2～118.93.1～10.273.3～110.11.9～9.0
菠菜83.4～118.71.5～7.991.0～117.73.8～11.072.7～119.14.1～10.6
牛油果73.2～118.92.4～9.974.8～117.04.4～11.980.5～117.64.9～11.0
黄豆芽97.2～118.83.4～12.076.0～118.01.8～9.971.4～118.91.7～10.1
), ArticleFig(id=1241680454735164106, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241522856148923206, language=CN, label=表2, caption=

不同加标水平和基质的回收率及相对标准偏差（%）

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称加标1（0.040 mg/kg）加标2（0.125 mg/kg）加标3（0.200 mg/kg）
平均回收率相对标准偏差平均回收率相对标准偏差平均回收率相对标准偏差
苹果80.5～117.32.6～9.694.3～114.61.6～6.675.0～111.82.2～9.7
黄瓜81.9～118.33.3～10.281.1～107.94.1～9.872.8～108.61.2～6.4
香蕉76.0～118.03.0～8.177.7～109.93.6～7.974.5～116.13.1～9.4
土豆73.8～113.92.3～9.574.3～103.22.1～7.672.0～100.23.8～12.0
草莓82.5～118.01.9～9.289.2～118.93.1～10.273.3～110.11.9～9.0
菠菜83.4～118.71.5～7.991.0～117.73.8～11.072.7～119.14.1～10.6
牛油果73.2～118.92.4～9.974.8～117.04.4～11.980.5～117.64.9～11.0
黄豆芽97.2～118.83.4～12.076.0～118.01.8～9.971.4～118.91.7～10.1
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QuEChERs结合气相色谱-串联质谱法测定不同果蔬基质中33种有机磷类农药残留量
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夏仕青 , 吴桃丽 , 薛云 , 李晓慧
现代预防医学 | 实验技术及其应用 2024,51(3): 523-528
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现代预防医学 | 实验技术及其应用 2024, 51(3): 523-528
QuEChERs结合气相色谱-串联质谱法测定不同果蔬基质中33种有机磷类农药残留量
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夏仕青 , 吴桃丽, 薛云, 李晓慧
作者信息
  • 贵州省黔西南州疾病预防控制中心监测检验科，贵州 兴义 562400

    • 夏仕青（1990—），女，硕士，主管技师及公卫医师，研究方向：环境及食品卫生检测

通讯作者:

夏仕青，E-mail：
Determination of 33 organophosphorus pesticide residues in different fruit and vegetable substrates by QuEChERs combined with gas chromatography-tandem mass spectrometry
Shi-qing XIA , Tao-li WU, Yun XUE, Xiao-hui LI
Affiliations
  • Department of Surveillance, Center for Disease Control and Prevention, Qianxinan Prefecture, Guizhou Province, Xingyi, Guizhou 562400, China
出版时间: 2024-02-10 doi: 10.20043/j.cnki.MPM.202308392
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摘要
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目的

采用QuEChERs前处理结合气相色谱-串联质谱技术，建立四种不同果蔬基质（普通型、高色素型、高脂肪型及高糖型）中33种有机磷类农药残留量快速检测方法，为不同水果、蔬菜中多种有机磷农药同时检测和食品安全风险评估提供技术支持。

方法

样品经乙腈及柠檬酸钠-柠檬酸氢二钠缓冲液同时提取，乙二胺-N-丙基硅烷（PSA）、十八烷基硅烷键合硅胶（C18）及石墨化炭黑（GCB）三种吸附剂净化，氮吹浓缩后用丙酮复溶，采用气相色谱-串联质谱仪在多反应离子监测(MRM)模式下进行检测，内标法定量。

结果

四种不同果蔬基质中33种有机磷类农药在50～500 μg/L的浓度范围内相关系数均大于0.995 0，方法检出限为1.50～5.04 μg/kg，定量限为5.01～16.78 μg/kg；在添加0.040～0.200 mg/kg水平范围内，农药的平均回收率为71.4%～119.1%，相对标准偏差均低于12%。

结论

该方法简单快速、准确度高、精密度好，适用于不同果蔬基质中33种有机磷类农药残留的快速检测和定量分析。

有机磷类农药  /  果蔬  /  QuEChERs  /  气相色谱-串联质谱法
Objective

To establish a rapid method for the determination of 33 organophosphorus pesticide residues in four different fruit and vegetable substrates (common type, high pigment type, high fat type, and high sugar type) by QuEChERs pretreatment combined with gas chromatography-tandem mass spectrometry (GC-MS), so as to provide technical support for simultaneous detection and food safety risk assessment of organophosphorus pesticides in different fruits and vegetables.

Methods

The samples were extracted with acetonitrile and sodium citrate-disodium hydrogen citrate buffer at the same time, purified with ethylenediamine-N-propyl silane (PSA), octadecylsilane bonded silica gel (C18), and graphitized carbon black (GCB). After nitrogen blowing concentration, the samples were re-dissolved with acetone and detected by gas chromatography-tandem mass spectrometry under multi-reaction ion monitoring (MRM) mode. Quantifications were based on internal standard curves.

Results

The method had good linear relationship in the range of 50 μg/L to 500 μg/L, with the correlation coefficients greater than 0.9950. The detection limits were within 1.50 to 5.04 μg/kg, and the limits of quantification were within 5.01 to 16.78 μg/kg. In the range of 0.040 to 0.200 mg/kg, the average recoveries ranged from 71.4% to 119.1%, with the relative standard deviations less than 12%.

Conclusion

The method is simple and rapid, with high accuracy and precision, which is suitable for the rapid detection and quantitative analysis of 33 organophosphorus pesticide residues in different fruit and vegetable substrates.

Organophosphorus pesticides  /  Fruits and vegetables  /  QuEChERs  /  Gas chromatography-tandem mass spectrometry
夏仕青, 吴桃丽, 薛云, 李晓慧. QuEChERs结合气相色谱-串联质谱法测定不同果蔬基质中33种有机磷类农药残留量. 现代预防医学, 2024 , 51 (3) : 523 -528 . DOI: 10.20043/j.cnki.MPM.202308392
Shi-qing XIA, Tao-li WU, Yun XUE, Xiao-hui LI. Determination of 33 organophosphorus pesticide residues in different fruit and vegetable substrates by QuEChERs combined with gas chromatography-tandem mass spectrometry[J]. Modern Preventive Medicine, 2024 , 51 (3) : 523 -528 . DOI: 10.20043/j.cnki.MPM.202308392
正文
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水果和蔬菜因各类杀虫剂、杀菌剂等在种植过程中的广泛使用，其农药残留造成的危害逐渐成为人们重点关注的食品安全问题[1-2]。其中有机磷类农药是我国使用广泛、用量最大的一类杀虫剂，其可通过抑制乙酰胆碱酶的活性，破坏乙酰胆碱的正常传导功能，从而导致机体出现一系列神经系统损害[3]。较多监测数据表明果蔬中农药残留总体超标率虽较低，但叶菜类蔬菜中有机磷农药检测率较其他蔬菜明显增高，且仍存在禁用农药使用的现象[4-5]。因此，建立高效、简便的果蔬中有机磷类农药多残留分析方法对及时了解果蔬中有机磷农药污染现状及针对性采取监管措施具有重要意义。
果蔬基质较复杂，其中色素、脂肪、糖分等组分是影响样品前处理效率及待测物准确定性定量的重要因素[6]。近年来，分散固相萃取（QuEChERS）方法因其简便、快速及高效等优点已逐渐成为果蔬中农药残留分析的优选前处理技术[7]，而气相色谱法-串联质谱法有效地利用了质谱鉴定能力和气相色谱高分离能力，可极大地提升多种有机磷类农药同时检测的精准度[8]。目前，虽已有部分学者研究报道了关于QuEChERs前处理结合气相色谱-串联质谱技术在水果、蔬菜中有机磷类农药的检测应用，但大多只采用了单一基质，如黄瓜[9]、苦瓜[10]及苹果[11]等对样品前处理条件进行优化及方法参数的验证，且提取、净化方法不尽一致；此外，少数学者只分析了豇豆[12]、大蒜[13]及猕猴桃[14]等某一类果蔬品种中有机磷农药的检测技术，研究结果代表性不足，不利于日常大批量不同基质类型的果蔬中有机磷农药的快速、准确定量。因此，本文以四种不同类型的果蔬基质，即普通型、高色素型、高脂肪型及高糖型为样品，优化了不同基质下提取溶剂、净化剂及仪器测定参数，建立QuEChERs前处理结合气相色谱-串联质谱测定不同果蔬基质中33种有机磷类农药残留量快速检测方法，以期为果蔬中有机磷类农药残留量的准确监测及风险评估提供参考。
1　材料与方法
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1.1　样品
四种不同类型的果蔬基质样品：普通型（苹果、黄瓜）、高色素型（草莓、菠菜）、高脂肪型（牛油果、黄豆芽）及高糖型（香蕉、土豆），采自黔西南州内农贸市场。样品取可食部分后，用匀浆机进行充分混匀，冷冻保存。
1.2　仪器与试剂
1.2.1 Trace 1300-TSQ8000 Evo气相色谱-质谱联用仪（美国Thermo公司）；BHL-2200H型分析天平（日本岛津有限公司）；UMV-2多管涡旋混合器（北京优晟联合科技有限公司）；H-1850R台式高速冷冻离心机（长沙湘仪公司）；AutoEVA-2plus全自动平行浓缩仪（曾科集团股份有限公司）；快速混匀器（heidolph公司）；Mili-Q纯水处理机（美国MILLIPORE有限公司）。
1.2.2 33种有机磷农药标准品（浓度均为1 000 mg/L，北京坛墨质检科技有限公司）；环氧七氯B内标（质量浓度为100 mg/L，北京坛墨质检科技有限公司）；乙腈（色谱纯，Puredil有限公司）；丙酮（色谱纯，西陇科
学股份有限公司）；乙酸（色谱纯，川东化工）；乙酸钠（分析纯，成都金山化学试剂有限公司）；柠檬酸钠（分析纯，天津市津科精细化工研究所）；柠檬酸氢二钠、氯化钠、无水硫酸镁（优级纯，成都艾克达化学试剂有限公司）；乙二胺-N-丙基硅烷(primary secondary amine, PSA) （深圳逗点生物公司）；十八烷基硅烷键合硅胶（C18）(Sigma-Aldrich公司)；石墨化碳黑（GCB，120～400目，天津博纳艾杰尔科技有限公司）。
1.3　标准溶液及内标的配制
1.3.1　33种有机磷类农药的混合标准溶液
分别吸取1.00 ml各标准储备液（1 000 mg/L）于100 ml容量瓶中，用丙酮定容至刻度，配制成10 mg/L的混合标准中间溶液；再吸取1.00 ml混合标准中间溶液（10 mg/L）于10 ml容量瓶中，用丙酮定容至刻度，配制成1.00 mg/L的混合标准使用溶液，在-20℃避光保存。
1.3.2　内标溶液
将环氧七氯B标准液（100 mg/L）用丙酮准确稀释20倍后，即浓度为5.00 mg/L的内标溶液。
1.3.3　基质混合标准工作溶液
空白基质溶液氮气吹干，加入30 μl内标溶液，加入1.00 ml相应质量浓度的混合标准溶液复溶后过微孔滤膜，现用现配。
1.4　仪器工作条件
1.4.1　气相色谱条件
HP-5 MS Ultra Inert色谱柱（30 m×250 μm，0.25 μm，美国Agilent公司）；柱温（升温程序）：40℃保持1.5 min，以25℃/min升温至90℃保持1.5 min，以25℃/min升温至180℃，再以5℃/min 升温至280℃，再以10℃/min 升温至300℃，保持5 min；运行时间35 min。载气为氦气（纯度≥99.999 %），流速1.0 ml/min。不分流进样，进样体积2 μl，进样口温度250℃，接口温度280℃。
1.4.2　质谱条件
离子源温度：300℃；传输线温度：280℃；电离模式：电子轰击电离(EI)；轰击能量：70 eV；灯丝电流：80μA；碰撞气：氩气（纯度≥99. 999%)；溶剂延迟时间：4.5 min；数据采集模式：多反应监测（MRM）。被监测离子及碰撞能量见表1。
1.5　样品的处理
准确称取10.00 g试样于50 ml塑料离心管中，加入10.0 ml乙晴、1.0 g柠檬酸钠、0.5 g柠檬酸氢二钠，盖上离心管盖，剧烈振荡5min后，加入1.0 g氯化钠后混匀1min，再加入4.0 g无水硫酸镁混匀2min，4 200 r/min离心5 min。吸取4.00 ml上清液加到内含900 mg无水硫酸镁、150 mgPSA、75 mgC18及15 mgGCB的15ml塑料离心管中，涡旋混匀1 min。4 200 r/min离心5 min，准确吸取2.00 ml上清于15 ml试管中，40℃水浴中氮气吹至近干。加入1.00 ml丙酮复溶，再加入30 μl的内标溶液，过微孔滤膜后上机测定。
2　结果
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2.1　有机磷农药保留时间及MRM质谱参数的确定
采用全扫描模式对33种有机磷农药及内标标准品溶液进行扫描，确定各农药的保留时间，并在各农药的质谱图中选取强度高且质荷比大的特征离子作为母离子，采用子离子扫描，对选定的母离子打碎，获得其子离子谱图，最后在MRM模式下优化所选子离子的最佳碰撞能量，结果见表1。各农药组分的MRM总离子流色谱见图1。
2.2　样品量的选择
文中考察了取样量为2.00、5.00、10.00和15.00 g时8种果蔬基质中33种有机磷有机农药回收率情况。结果表明，与取5.00 g样品相比，当取10.00 g样品分析时8种果蔬基质中回收率为70%～120%的农药组分占农药总数的平均比例明显提高，可达82.2%。而取样量过低（2.00 g）或过高（15.00 g）时，可引起农药回收率波动大，结果不稳定或必须加大萃取剂及净化剂量等问题。故取样量为10.00 g。
2.3　提取溶剂的优化
农残分析中，选择合适的提取剂是提高检测准确度及精密度的关键。研究表明，乙腈因其极性较强，对农残具有较高的提取效率并能有效减少油脂、色素等对农药的干扰；此外，通过加入乙酸盐或柠檬酸钠及柠檬酸氢二钠缓冲盐使样品提取液处于偏酸状态，可明显提高酸碱敏感性农药的回收率[15]。因此，本文在空白苹果、菠菜和黄豆芽等8种果蔬样品中分别添加0.200 mg/kg的33种有机磷农药混合标准溶液，对比分析了3种提取方法的提取效率，即：（1）直接用乙腈提取；（2）采用10 ml乙腈 + 1.0 g柠檬酸钠 + 0.5 g柠檬酸氢二钠缓冲体系提取；（3）采用10 ml 1%乙酸乙腈 + 1.5 g乙酸钠缓冲体系进行提取。由图2可知，当采用方法（2）提取时，33种有机磷农药在8种果蔬基质中均有较好回收率，回收率在70%～120%之间的农药组分最多，占农药总数的89.4%，说明该方法的萃取效果最好。因此，实验选择乙腈+柠檬酸钠+柠檬酸氢二钠缓冲体系进行提取。
2.4　净化剂的选择
QuEChERS法常用的净化剂有PSA、C18及GCB等。其中，PSA可有效除去基质中的糖类、脂肪酸和甾醇等成分；C18主要用于吸附基质中的脂肪、脂溶性维生素等；而GCB除色素、维生素的能力较好，但对含有芳香环、结构具有一定对称性的农药有较强的吸附作用[16]。通过在8种果蔬样品的空白提取液中分别添加0.200 mg/kg的33种有机磷农药混合标准溶液，对比分析了6种提取方法的农药回收率情况。包括（1）900 mg无水硫酸镁 + 150 mgPSA；（2）900 mg无水硫酸镁 + 150 mgPSA + 15 mgGCB；（3）900 mg无水硫酸镁 + 150 mgPSA + 75 mgC18；（4）900 mg无水硫酸镁 + 150 mgPSA + 75 mgC18 + 15 mgGCB；（5）900 mg无水硫酸镁 + 150 mgPSA + 100 mgGCB；（6）900 mg无水硫酸镁 + 150 mgPSA + 75 mgC18 + 100 mgGCB。由图3可知，浅色或无色样品基质样品（如苹果、黄瓜、土豆等）采用方法（1）、（3）、（4）进行净化时，大多数农药具有较好的回收率，而随着GCB含量的提高，回收率为70%～120%的农药组分占农药总数的比例显著降低。深色样品（如菠菜、草莓、牛油果等）在GCB含量为15 mg时具有较好回收率，随着GCB含量提高到100 mg时，提取溶液呈澄清透明，但回收率为70%～120%的农药组分占农药总数的比例明显降低。6种净化方法下回收率为70%～120%的农药组分占农药总数的平均比例分别为60.2%、86.4%、72.7%、92.4%、45.1%、51.1%，即采用方法（4）净化时，8种果蔬样品的净化效果最好，回收率在70%～120%之间的农药组分最多。因此，实验选择900 mg无水硫酸镁+ 150 mgPSA+75 mgC18+15 mgGCB对不同果蔬样品进行净化。
2.5　基质效应的考察
采用标准曲线斜率比较法考察了33种有机磷农药在8种不同样品中的基质效应(matrix effect, ME)，即ME(%) = (B/A-1) × 100，其中B为基质标准曲线斜率，A为溶剂标准曲线斜率。当ME绝对值小于20%时，表现为弱基质效应；20%～50%表现为中等基质效应；而大于50%时表现为较强的基质效应[17]。结果显示，8种果蔬样品中基质效应大于50%的有机磷农药组分占农药总数的比例为45.5%～100%，提示大多数有机磷农药在果蔬中均表现为中强基质效应，这与许炳雯等[17]研究报道一致。因此，为了校正基质效应的影响，实验中采用基质配制标准曲线，内标法进行定量。
2.6　方法线性范围和检出限
在空白苹果、菠菜和黄豆芽等8种不同基质样品中准确配制含量为0.05、0.10、0.15、0.20、0.25、0.30、0.35、0.40、0.45和0.50 mg/L的混合标准系列溶液，本法分析后，以组分的质量浓度为横坐标，峰面积与内标峰面积比值为纵坐标绘制标准工作曲线，并以各目标物在阴性样品中的3倍、10倍信噪比分别计算方法的检出限及定量限。结果表明，33种有机磷农药在50～500 μg/L的浓度范围内有良好的线性关系，相关系数为0.995 4～0.999 2，方法检出限为1.50～5.04 μg/kg，定量限为5.01～16.78 μg/kg，均低于0.02 mg/kg。
2.7　方法加标回收率及精密度
在不同基质空白样品中分别加入3个不同浓度的混合标准溶液（加标后含量分别为0.040、0.125和0.200 mg/kg）。放置过夜后，按本法进行平行6次测定，以分析不同基质下方法的加标回收率及精密度情况。结果表明，在3个加标水平下的平均回收率为71.4%～119.1%，相对标准偏差均低于12%。见表2。
2.8　实际样品的检测
将本实验建立的方法应用于韭菜、菠菜、土豆、黄豆芽、黄瓜、西红柿等46份蔬菜以及苹果、香蕉、火龙果、草莓、猕猴桃等13份水果，共59份，结果显示，1份香菜检出乙酰甲胺磷，1份圆白菜检出喹硫磷农药残留，其他样品均未检出相应农药。
3　结论
收起
本文采用QuEChERS结合气相色谱-串联质谱技术测定了不同基质类型的水果、蔬菜中33种有机磷类农药，通过优化样品提取、净化及仪器工作条件，有效简化了操作流程，建立了不同果蔬样品中有机磷农药残留的气质联用法定性定量分析方法。该方法简单快速、灵敏度高、重现性较好，适用于大批量不同果蔬基质中有机磷类农药残留检测，为果蔬产品中农药残留污染的安全风险评估工作提供了技术支持。
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2024年第51卷第3期
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doi: 10.20043/j.cnki.MPM.202308392
  • 接收时间：2023-08-20
  • 首发时间：2026-03-19
  • 出版时间：2024-02-10
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  • 收稿日期：2023-08-20
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    贵州省黔西南州疾病预防控制中心监测检验科，贵州 兴义 562400

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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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