Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction

BI Jun; REN Jun; ZHAO Yun-feng; CHEN Da-wei

doi:10.19969/j.fxcsxb.20123108

您当前的位置：

首页 >

文章列表页 >

Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction

Scientific Papers | 更新时间：2023-02-13

- Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction
- Journal of Instrumental Analysis Vol. 40, Issue 9, Pages: 1318-1327(2021)
- 作者机构：
  
  1.国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室，北京 100021
  2.盘锦检验检测中心，辽宁盘锦 124000
  3.乌海市检验检测中心，内蒙古乌海 016000
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.20123108
  CLC：
扫描看全文
毕军,任君,赵云峰等.QuEChERS－冷冻诱导液液萃取/液相色谱－高分辨质谱法测定蔬菜水果中77种农药残留[J].分析测试学报,2021,40(09):1318-1327.

BI Jun,REN Jun,ZHAO Yun-feng,et al.Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction[J].Journal of Instrumental Analysis,2021,40(09):1318-1327.
毕军,任君,赵云峰等.QuEChERS－冷冻诱导液液萃取/液相色谱－高分辨质谱法测定蔬菜水果中77种农药残留[J].分析测试学报,2021,40(09):1318-1327. DOI： 10.19969/j.fxcsxb.20123108.

BI Jun,REN Jun,ZHAO Yun-feng,et al.Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction[J].Journal of Instrumental Analysis,2021,40(09):1318-1327. DOI： 10.19969/j.fxcsxb.20123108.

摘要

基于QuEChERS－冷冻诱导液液萃取（CI－LLE）技术，建立了蔬菜水果中77种农药残留的超高效液相色谱－高分辨质谱检测方法。样品经常规QuEChERS方法提取、盐析和净化后，进一步以40%乙腈－水溶液对77种农药进行CI－LLE富集和净化。仪器分析以水－甲醇（两相中均含0.1%甲酸和4 mmol/L甲酸铵）为流动相进行梯度洗脱，C,18,色谱柱（2.6 μm，2.1 mm × 150 mm）分离，高分辨质谱以时间分段全扫描模式采集，内标法定量。结果显示，77种农药在一定浓度范围内呈良好的线性关系（,r,2,>, 0.99）；方法检出限为0.02～0.20 μg/kg，定量下限为0.05～0.50 μg/kg。空白样品在4个不同加标水平的回收率为70.8%～119%，相对标准偏差（RSD）为0.70%～15%。该方法操作简单，重现性好，能降低基质效应对农残检测的影响，具有较高的灵敏度、准确度和精密度，符合农药多残留检测技术的要求，已应用于实际样品中农药残留的定性和定量分析。

Abstract

Based on QuEChERS and cold induced liquid－liquid extraction（CI－LLE） technique， an analytical method for the determination of 77 pesticide residues in vegetables and fruits was developed by ultra-high performance liquid chromatography－high resolution mass spectrometry. The samples were extracted， salted out， and cleaned up by traditional QuEChERS method， and further enriched and cleaned up by CI－LLE technique using 40% acetonitrile－water solution. The chromatographic separation of pesticides was performed on a C,18, column（2.1 mm × 150 mm， 2.6 μm） using water－methanol （containing 0.1% formic acid and 4 mmol/L ammonium formate for each） as mobile phases by gradient elution. The pesticides were analyzed by the high resolution mass spectrometry in full scan mode by time sediment， and quantified by internal standard method. Results showed that 77 pesticides had good linearity in the certain concentration ranges with relative coefficients（,r,2,） larger than 0.99. The limits of detection and limits of quantitation were in the ranges of 0.02－0.20 μg/kg and 0.05－0.50 μg/kg， respectively. At four different spiked levels， the recoveries for pesticides in vegetables and fruits ranged from 70.8% to 119%， with relative standard deviations（RSDs） of 0.70%－15%. The method is simple and reproducible， and could be used to reduce matrix effect on the detection of pesticide residues with high sensitivity， accuracy， and precision. Therefore， it could meet the requirements for multi-residue detection of pesticides， and be applied to the qualitative and quantitative determination of pesticides in real samples.

关键词

农药残留冷冻诱导液液萃取高分辨质谱蔬菜水果QuEChERS

Keywords

pesticide residuescold induced liquid－liquid extractionhigh resolution mass spectrometryvegetablesfruitsQuEChERS

references

European Food Safety Authority. Review of the Existing Maximum Residue Levels for Clothianidin According to Article 12 of Regulation （EC） No 396/2005［2019－05－22］. https：//efsa.onlinelibrary. wiley. com/doi/full/10.2903/j. efsa. 2019https://efsa.onlinelibrary.wiley.com/doi/full/10.2903/j.efsa.2019.

Food and Drug Administration. Pesticide Residue Monitoring 2015 Report and Data［2017－11－01］. https：//www.fda.gov/food/pesticides/pesticide－residue－monitoring－2015－report－and－datahttps://www.fda.gov/food/pesticides/pesticide-residue-monitoring-2015-report-and-data.

Bundesinstitut Für Risikobewertung. Proposal for an Assessment Concept for Pesticides with Adverse Effects on the Human Endocrine System［2010－04－19］. https：//www.bfr.bund.de/cm/343/proposal for an assessment concept for pesticideshttps://www.bfr.bund.de/cm/343/proposalforanassessmentconceptforpesticides.

GB 2763－2019. 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）.

Yang Y H， Kong W J， Zhao L H， Xiao Q， Liu H M， Zhao X S， Yang M H. J. Chromatogr. B， 2015， 974： 118－125.

Tuzimski T， Rejczak T. Food Chem.， 2016， 190： 71－79.

Lee H S， Rahman M M， Chung H S， Kabir H， Yoon K S， Cho S K， EI－Aty A M A， Shim J H. J. Chromatogr. B， 2018， 1095： 1－7.

Zhang F， Zhang Y， Huang Z Q， Bai S， Xi H， Cai Q Y. J. Instum. Anal. （张帆，张莹，黄志强，白珊，席慧，蔡青云. 分析测试学报）， 2019， 38（4）： 411－416.

Choi S， Kim S， Shin J Y， Kim M K， Kim J H. Food Chem.， 2015， 173： 1236－1242.

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.

Timofeeva I， Shishov A， Kanashina D， Dzema D， Bulatov A. Talanta， 2017， 167： 761－767.

Mérillon J M， Ramawat K. Bioactive Molecules in Food. Switzerland: Springer， Cham.， 2019.

Concha－meyer A， Grandon S， Sepúlveda G， Diaz R， Yuri J A， Torres C. Food Chem.， 2019， 295： 64－71.

Lawal A， Wong R C S， Tan G H， Abdulrauf L B， Alsharif A M A. J. Chromatogr. Sci.， 2018， 56（7）： 656－669.

Cao X Y， Chen S G， Zeng C Y， Li X J， Wang L. J. Instum. Anal. （曹小云，陈树干，曾楚莹，黎秀娟，王露. 分析测试学报）， 2019， 38（8）： 920－930.

Rizzetti T M， Kemmerich M， Martins M L， Prestes O D， Adaime M B， Zanella R. Food Chem.， 2016， 196： 25－33.

Ding L P， Cai C P， Wang D H. Chin. J. Chromatogr.（丁立平，蔡春平，王丹红. 色谱）， 2014， 32（8）： 849－854.

Li S H， Chen D W， Lü B， Li J G， Zhao Y F， Wu Y N. J. Agric. Food Chem.， 2019， 67： 2732－2740.

Li S H， Ren J， Zhang Y P， Li L F， Zhao Y F， Chen D W， Wu Y N. Food Chem.， 2020， 328： 127113.

Wang F Q， Li S H， Feng H， Yang Y J， Xiao B， Chen D W. Food Chem.， 2019， 275： 530－538.

Chen D W， Gao J， Lü B， Zhu P， Yang X， Zhao Y F， Miao H. Chin. J. Anal. Chem.陈达炜，高洁，吕冰，朱盼，杨欣，赵云峰，苗虹. 分析化学）， 2014， 42（4）： 579－584.

Views

下载量

CSCD

Alert me when the article has been cited

提交

Tools

Publicity Resources

Determination of 67 Pesticide Residues in Vegetables and Fruits by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Dispersive Solid Phase Extraction

Determination of 50 Common Pesticide Residues in Golden Siraitia Grosvenoriis by QuEChERS and High Performance Liqiud Chromatography－Tandem Mass Spectrometry

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

Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage

Determination of 232 Pesticide Residues in Dairy Products by Gas Chromatography－Tandem Mass Spectrometry

Related Author

No data

Related Institution

东莞市农产品质量安全监督检测所

Guangzhou Institute for Drug Control，NMPA Key Laboratory for Quality Evaluation of Traditional Medicine

Hanzhong Food and Drug Supervision，Inspection and Testing Center，Shaanxi Tea Products Quality Supervision and Inspection Center

Chenggu Food and Drug Inspection and Testing Center

Pesticide Safety Evaluation Research Center，Institute for Agro-food Standards and Testing Technology，Shanghai Academy of Agricultural Sciences

Address：100 Xianlie Middle Road, Guangzhou Postal code：510070
Tel：020-87684776,37656606 Fax：020-87684776 Email：fxcsxb@china.com
Technical support is provided by Beijing Founder electronics co., LTD 粤ICP备12017312号-3 京公网安备11010802024621
It is recommended to read the content of this site in Chrome&IE9+. Please switch to extreme mode in browser 360.
Cookies We use cookies to help provide and enhance our service and tailor content. By continuing, you agree to the use of cookies.

⁰