Determination of 37 Pesticide Residues in Tea by Gas Chromatography－Tandem Mass Spectrometry Combined with QuEChERS and Prepositive Internal Standard

HUANG Wei; MA Yu-feng; MENG Yi-fan; LI Chong-yong; LI Chun-mei; LI Ting; WANG Yu-xin; DING Wei

doi:10.19969/j.fxcsxb.22031607

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Determination of 37 Pesticide Residues in Tea by Gas Chromatography－Tandem Mass Spectrometry Combined with QuEChERS and Prepositive Internal Standard

Experimental Techniques and Methods | 更新时间：2023-01-04

- Determination of 37 Pesticide Residues in Tea by Gas Chromatography－Tandem Mass Spectrometry Combined with QuEChERS and Prepositive Internal Standard
- Journal of Instrumental Analysis Vol. 41, Issue 8, Pages: 1221-1228(2022)
- 作者机构：
  
  1.陕西省茶叶产品质量监督检验中心汉中市食品药品监督检验检测中心，陕西汉中 723000
  2.城固县食品药品检验检测中心，陕西汉中 723200
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22031607
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黄微,马玉凤,孟怡璠等.QuEChERS/气相色谱－串联质谱－内标前置法测定茶叶中37种农药残留[J].分析测试学报,2022,41(08):1221-1228.

HUANG Wei,MA Yu-feng,MENG Yi-fan,et al.Determination of 37 Pesticide Residues in Tea by Gas Chromatography－Tandem Mass Spectrometry Combined with QuEChERS and Prepositive Internal Standard[J].Journal of Instrumental Analysis,2022,41(08):1221-1228.
黄微,马玉凤,孟怡璠等.QuEChERS/气相色谱－串联质谱－内标前置法测定茶叶中37种农药残留[J].分析测试学报,2022,41(08):1221-1228. DOI： 10.19969/j.fxcsxb.22031607.

HUANG Wei,MA Yu-feng,MENG Yi-fan,et al.Determination of 37 Pesticide Residues in Tea by Gas Chromatography－Tandem Mass Spectrometry Combined with QuEChERS and Prepositive Internal Standard[J].Journal of Instrumental Analysis,2022,41(08):1221-1228. DOI： 10.19969/j.fxcsxb.22031607.

摘要

采用QuEChERS前处理技术，结合内标前置法建立了气相色谱－串联质谱同时检测茶叶中37种农药残留的方法，待测农药包括14种有机磷类、10种有机氯类、8种拟除虫菊酯类和5种有机杂环类。比较了提取溶剂、加水量、内标放置方式对37种农药提取效果的影响，考察了不同类型茶叶的基质效应，确定最优的实验条件为：茶叶样品加入内标后，加水浸泡，经乙腈超声提取，QuEChERS法净化，采用气相色谱－串联质谱仪多反应离子监测模式（MRM）进行检测，基质匹配标准曲线内标法定量。结果表明：内标前置法比内标后置法的回收率高，绿茶、红茶、白茶、黑茶基质均以基质增强效应为主。在优化实验条件下，37种农药在相应的质量浓度范围内呈良好的线性关系，相关系数（,r,2,）均大于0.99。方法检出限（LOD）为0.2～15.7 μg/kg，定量下限（LOQ）为0.7～52.2 μg/kg。37种农药在LOQ、2LOQ和10LOQ 3个加标水平下的回收率为70.2%～120%，相对标准偏差（RSD）为1.1%～11%。该方法操作简单、准确高效、成本较低，适用于茶叶中农药多残留的日常检测。

Abstract

A gas chromatography－tandem mass spectrometry（GC－MS/MS） combined with QuEChERS plus prepositive internal standard was developed for the simultaneous detection of 37 pesticide residues in tea. The target pesticides included 14 organophosphorus pesticides，10 organochlorine pesticides，8 pyrethroid pesticides and 5 organic heterocyclic pesticides. The effects of different extraction solvents，water amounts and internal standard adding approaches on extraction were studied. The matrix effects of 37 pesticides in different types of tea were also explored. The optimal experimental conditions were as follows：firstly，the tea samples were soaked for 30 min with 10 mL water after adding heptachlor epoxide as internal standard，then the target pesticides were extracted ultrasonically using 20 mL acetonitrile for 20 min，followed by adding QuEChERS extract pouch（containing 6 g magnesium sulfate and 1.5 g sodium acetate）. After vortexing evenly and centrifugation，10 mL of the supernatant was separated and transferred into QuEChERS purge tube which contained a mixed sorbent of 1 200 mg magnesium sulfate，400 mg primary secondary amine（PSA），400 mg C,18, and 400 mg graphitized carbon black（GCB）. The mixtures were vortexed evenly and centrifugated. Then 2 mL of the purified solution was concentrated by nitrogen blowing at 40 ℃ until the solution was nearly desiccated. After that，1 mL ethyl acetate was used to redissolve the residues. Finally，the target pesticides were detected by GC－MS/MS in multiple reaction monitoring（MRM） mode，and quantified by the internal standard method with matrix matching standard curve. The results showed that the use of prepositive internal standard had a better recovery result than the use of postpositive internal standard. Chromatogram signals of most pesticides in green tea，black tea，white tea and dark tea matrices were enhanced distinctly. Under the optimized conditions，good linear relationships were observed for the 37 pesticides，and the correlation coefficients（,r,2,） were greater than 0.99. The limits of detection（LODs） and the limits of quantitation（LOQs） were in the range of 0.2－15.7 μg/kg and 0.7－52.2 μg/kg，respectively. The recoveries for 37 pesticides at three spiked levels（the LOQ，2 times the LOQ and 10 times the LOQ） ranged from 70.2% to 120%，with relative standard deviations（RSDs） of 1.1%－11%. This method has the features of simple operation，high accuracy，high efficiency and low cost，which could be applied to the routine detection of pesticide residues in tea.

关键词

气相色谱－串联质谱QuEChERS内标前置茶叶农药残留

Keywords

gas chromatography－tandem mass spectrometry（GC－MS/MS）QuEChERSprepositive internal standardteapesticide residues

references

Sun R，Yang W Q，Li Y X，Sun C J．Eur. Food Res. Technol.，2021，247：1839－1858.

Li X，Zhang Z W，Li P W，Zhang Q，Zhang W，Ding X X．Food Res. Int.，2013，53（2）：649－658.

Liu T F，Dong M H，Yang D F，Zhang C Z，Gu J R，Xu D L．Food Sci. （刘腾飞，董明辉，杨代凤，张存政，顾俊荣，徐德良．食品科学），2018，39（9）：310－325.

GB 2763－2021．National Food Safety Standard－Maximum Residue Limits for Pesticides in Food. National Standards of the People's Republic of China（食品安全国家标准食品中农药最大残留限量．中华人民共和国国家标准）.

Zhang F，Zhang X Z，Luo F J，Chen Z M，Sun W J，Liu G M，Lou Z Y．J. Instrum. Anal. 张芬，张新忠，罗逢健，陈宗懋，孙威江，刘光明，楼正云．分析测试学报），2013，32（4）：393－400.

Rong J F，Wei H，Huang H S，Li Y J，Xu M Z．J. Instrum. Anal. （荣杰峰，韦航，黄伙水，李亦军，许美珠．分析测试学报），2016，35（1）：5－15.

Zhu B Q，Jin S Q，Tian C X，Hu F，Xu X Y，Luo J W．J. Instrum. Anal. （朱炳祺，金绍强，田春霞，胡帆，徐潇颖，罗金文．分析测试学报），2018，37（4）：404－410.

Wang X L，Mao W Z，Wang X H，Lou C L，Wu F，Lu J L，Zhou X．Sci. Technol. Food Ind. 王晓亮，毛卫中，汪新华，楼春兰，吴飞，陆君羚，周璇．食品工业科技），2018，39（14）：190－193.

Meng X D，Song W，Xiao Y，Zheng P，Cui C J，Gao W J，Hou R Y．Food Chem.，2022，370：130846.

Jiao H Z，Lu S Q，Hou D，Zhang Q Q．Chin. J. Chromatogr. （焦慧泽，陆世清，侯迪，张前前．色谱），2019，37（6）：605－611.

Wu Y L，An Q S，Li D，Kang L，Zhou C R，Zhang J B．Food Chem.，2022，375：131819.

GB 23200.113－2018．National Food Safety Standard－Determination of 208 Pesticides and Metabolites Residues in Foods of Plant Origin－Gas Chromatography－Tandem Mass Spectrometry Method. National Standards of the People's Republic of China（食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱－质谱联用法．中华人民共和国国家标准）.

Huang W，Li N，Xu R H，Li T，Li C Y．Chin. J. Chromatogr. （黄微，李娜，徐瑞晗，李婷，李崇勇．色谱），2018，36（12）：1303－1310.

Li J X，Zhang Z J，Sun M Y，Zhang B L，Fan C L．Chromatographia，2018，81（5）：809－821.

Zhu B Q，Xu X Y，Luo J W，Jin S Q，Chen W Q，Liu Z，Tian C X．Food Chem.，2019，276：202－208.

Lin T，Chen X L，Guo J，Li M X，Tang Y F，Li M X，Li Y G，Cheng L，Liu H C．Molecules，2022，27（3）：1053－1067.

Xu Z Y，Xiao X，Jiang X B，Cai P M．Appl. Ecol. Env. Res.，2021，19（2）：1517－1532.

GB 23200.121－2021．National Food Safety Standard－Determination of 331 Pesticides and Metabolites Residues in Foods of Plant Origin－Liquid Chromatography－Tandem Mass Spectrometry Method. National Standards of the People's Republic of China（食品安全国家标准植物源性食品中331种农药及其代谢物残留量的测定液相色谱－质谱联用法．中华人民共和国国家标准）.

Yarita T，Aoyagi Y，Otake T．J. Chromatogr. A，2015，1396：109－116.

GB/T 27404－2008．Criterion on Quality Control of Laboratories－Chemical Testing of Food. National Standards of the People's Republic of China（实验室质量控制规范食品理化检测．中华人民共和国国家标准）.

Cao X Y，Pang G F，Jin L H，Kang J，Hu X Y，Chang Q Y，Wang M L，Fan C L．Chin. J. Chromatogr.

曹新悦，庞国芳，金铃和，康健，胡雪艳，常巧英，王明林，范春林．色谱），2015，33（4）：389－396.

Gao Y X，Chen P H，Nie D D．Chin. J. Chromatogr. （高艺羡，陈萍虹，聂丹丹．色谱），2018，36（6）：531－540.

Su J F，Zhong M S，Chen J，Guo X，Chen J X，Liang Z，Liu J J．J. Instrum. Anal. 苏建峰，钟茂生，陈晶，郭昕，陈劲星，梁震，刘建军．分析测试学报），2015，34（6）：625－638.

Yin X Y，Zhu J M，Du Y Y，Wang J Q，Zhai Y Z．J. Instrum. Anal. （殷雪琰，朱佳明，堵燕钰，王洁琼，翟云忠．分析测试学报），2022，41（2）：172－186.

Ye J L，Jin G E，Wu Y H，Zheng W H．Food Sci. （叶江雷，金贵娥，吴云辉，郑文慧．食品科学），2013，34（12）：265－271.

Man H P，Lü S，Mao J C，Che T，Luo Z G，Jiang D H，Zhou L．J. Food Saf. Qual. 满红平，吕生，毛静春，车涛，罗正刚，姜东华，周利．食品安全质量检测学报），2019，10（9）：2703－2722.

Chen H P，Liu X，Wang Q H，Jiang Y．Chin. J. Chromatogr. （陈红平，刘新，汪庆华，蒋迎．色谱），2011，29（5）：409－416.

Wang J L，Zeng H Y，Li S S，Zhang X L，Ma H C．J. Food Saf. Qual. （王家磊，曾海英，李思思，张晓丽，马洪超．食品安全质量检测学报），2021，12（7）：2582－2590.

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