Citation: LIU Yong, TANG Yingfei, SONG Jinfeng, HU Zhiwei. Determination of four organophosphorus pesticides and their metabolites in vegetables using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(2): 139-144. doi: 10.3724/SP.J.1123.2013.10008 shu

Determination of four organophosphorus pesticides and their metabolites in vegetables using solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry

LIU Yong ^1,2 ,
TANG Yingfei ^2,3 ,
SONG Jinfeng ^2,, ,
HU Zhiwei ²

1.
1. Technology Center of Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China;

Corresponding author: SONG Jinfeng,
Received Date: 11 October 2013
Available Online: 18 December 2013
Fund Project: 国家质检总局课题(2009IK177). (2009IK177)

Organophosphorus pesticides (OPs), malathion, methyl parathion, trichlorfon, and acephate were used frequently in vegetable cultivation, mainly metabolized into O,O-dimethyl dithiophosphate, 4-nitrophenol, dimethyl dichloroviny phosphate (DDVP) and methamidophos, respectively. A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of the organophosphorus pesticides and their metabolites. According to the difference of coloring matter contents in vegetable matrix, the pre-treatment for vegetables with high coloring matter contents were performed using activated carbon coupled with a Florisil solid-phase extraction column, and others were purified by a Florisil solid-phase extraction column. A hydrophilic interaction chromatographic column (ACQUITY UPLC BEH HILIC) was used with acetonitrile-5 mmol/L ammonium acetate as mobile phases. The MS/MS detection was performed under positive or negative electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The results showed that the matrix effect of the LC-MS/MS was 15.3%-45.1%, the recoveries of the four organophosphorus pesticides and their metabolites were 76.9%-102.8%, the precision ranged from 5.92% to 10.19%, the limits of quantification ranged from 0.001 to 0.01 mg/L, and the linear correlation coefficients were 0.9982-0.9999 in the range of 0.01-1.00 mg/L. This method was applied in the analysis of Chinese cabbages, hot peppers, tomatoes and onions from markets. This method can be applied in rapid detection of the organophosphorus pesticides and their metabolites in vegetables.
- solid-phase extraction (SPE),
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- organophosphorus pesticides,
- metabolites,
- vegetables
1. [1]
  [1] Zhang Q. Guangdong Chemical Industry (张强. 广东化工), 2013, 40(10): 142
2. [2]
  [2] Wang J, Zheng X Y. Science & Technology Association Forum (王晶, 郑晓燕. 科协论坛), 2013(4): 89
3. [3]
  [3] Jin T M, Sun X H. Journal of Inner Mongolia University for Nationalities (金天明, 孙晓辉. 内蒙古民族大学学报: 自然科学版), 2002, 17(5): 420
4. [4]
  [4] Kong Z Q, Dong F S, Xu J, et al. Food Control, 2012, 23(1): 149
5. [5]
  [5] Chávez-López C, Blanco-Jarvio A, Luna-Guido M, et al. Eur J Soil Biol, 2011, 47: 264
6. [6]
  [6] Loewenherz C, Fenske R A, Simcox N J, et al. Environ Health Perspect, 1997, 105(12): 1344
7. [7]
  [7] Lin W X. The Compilation of Residue Limits Standards for Pesticides and Veterinary Drugs in Foodstuffs in the World (林维宣. 各国食品中农药兽药残留限量规定. 大连: 大连海事大学出版社), 2003
8. [8]
  [8] Liu X P, Mitrevski B, Li D K, et al. Microchem J, 2013, 111(7): 25
9. [9]
  [9] Rodrigues F de M, Mesquita P R R, de Oliveira L S, et al. Microchem J, 2011, 98(1): 56
10. [10]
  [10] Chen X S, Bian Z Y, Yang F, et al. Chinese Journal of Chromatography (陈晓水, 边照阳, 杨飞, 等. 色谱), 2013, 31(11): 1116
11. [11]
  [11] Xu Z L, Deng H, Deng X F, et al. Food Chem, 2012, 131(4): 1569
12. [12]
  [12] Cao L W, Liang S L, Tan X F, et al. Chinese Journal of Chromatography (曹丽伟, 梁丝柳, 谭小芳, 等. 色谱), 2012, 30(12): 1295
13. [13]
  [13] Wang L Z, Zhou Y, Chen Y, et al. Chinese Journal of Chromatography (王连珠, 周昱, 陈泳, 等. 色谱), 2012, 30(2): 146
14. [14]
  [14] Song W, Lin S S, Sun G D, et al. Chinese Journal of Chromatography (宋伟, 林姗姗, 孙广大, 等. 色谱), 2012, 30(3): 318
15. [15]
  [15] Jiang S X, Feng J J. Chinese Journal of Chromatography (蒋生祥, 冯娟娟. 色谱), 2012, 30(3): 219
16. [16]
  [16] Wu C H, Zheng L X, Zhou Z J. Fudan Univ J: Med Sci (邬春华, 郑力行, 周志俊. 复旦学报: 医学版), 2006, 33(4): 552
17. [17]
  [17] Huang Y, Li Z Y, Zhao B S. Environmental Science and Management (黄雅, 李政一, 赵博生. 环境科学与管理), 2009, 34(4): 20
18. [18]
  [18] Liu Y, Yang C Z, Kang Q H, et al. Chinese Journal of Analysis Laboratory (刘永, 杨长志, 康庆贺, 等. 分析试验室), 2008, 27(2): 119
1. [1]
  Qilong Fang , Yiqi Li , Jiangyihui Sheng , Quan Yuan , Jie Tan . Magical Pesticide Residue Detection Test Strips: Aptamer-based Lateral Flow Test Strips for Organophosphorus Pesticide Detection. University Chemistry, 2024, 39(5): 80-89. doi: 10.3866/PKU.DXHX202310004
2. [2]
  Siwei Hou , Yaxin Niu , Guanglu Zhang , Yanmei Yang , Xu Wang , Zhenzhen Chen . Application of Solid-Phase Microextraction and Mass Spectrometry in Environmental Detection. University Chemistry, 2026, 41(3): 297-306. doi: 10.12461/PKU.DXHX202504078
3. [3]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
4. [4]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
5. [5]
  Junyuan Zhang , Zhiwei Miao . 有机磷杀虫剂的前世今生. University Chemistry, 2025, 40(6): 129-138. doi: 10.12461/PKU.DXHX202408118
6. [6]
  Haiyuan Wang , Xiaoning Jin , Yajing Sun , Zhen Zhang , Wentao Zhao , Yi Li . Practical Exploration of High-Performance Liquid Chromatography Experiment Teaching Reform Empowered by Artificial Intelligence. University Chemistry, 2026, 41(4): 45-51. doi: 10.12461/PKU.DXHX202505076
7. [7]
  Yifan Xie , Liyun Yao , Ruolin Yang , Yuxing Cai , Yujie Jin , Ning Li . Exploration and Practice of Online and Offline Hybrid Teaching Mode in High-Performance Liquid Chromatography Experiment. University Chemistry, 2025, 40(11): 100-107. doi: 10.12461/PKU.DXHX202412133
8. [8]
  Mingyang Men , Jinghua Wu , Gaozhan Liu , Jing Zhang , Nini Zhang , Xiayin Yao . Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries. Acta Physico-Chimica Sinica, 2025, 41(1): 100004-0. doi: 10.3866/PKU.WHXB202309019
9. [9]
  Shunü Peng , Huamin Li , Zhaobin Chen , Yiru Wang . Simultaneous Application of Multiple Quantitative Analysis Methods in Gas Chromatography for the Determination of Active Ingredients in Traditional Chinese Medicine Preparations. University Chemistry, 2025, 40(10): 243-249. doi: 10.12461/PKU.DXHX202412043
10. [10]
  Qianlang Wang , Jijun Sun , Qian Chen , Quanqin Zhao , Baojuan Xi . The Appeal of Organophosphorus Compounds: Clearing Their Name. University Chemistry, 2025, 40(4): 299-306. doi: 10.12461/PKU.DXHX202405205
11. [11]
  Fengxiao Wang , Zhiwei Miao , Yaofeng Yuan . 有机磷化学与化学教学. University Chemistry, 2025, 40(8): 158-168. doi: 10.12461/PKU.DXHX202410077
12. [12]
  Chongjing Liu , Yujian Xia , Pengjun Zhang , Shiqiang Wei , Dengfeng Cao , Beibei Sheng , Yongheng Chu , Shuangming Chen , Li Song , Xiaosong Liu . Understanding Solid-Gas and Solid-Liquid Interfaces through Near Ambient Pressure X-Ray Photoelectron Spectroscopy. Acta Physico-Chimica Sinica, 2025, 41(2): 100013-0. doi: 10.3866/PKU.WHXB202309036
13. [13]
  Runjie Li , Hang Liu , Xisheng Wang , Wanqun Zhang , Wanqun Hu , Kaiping Yang , Qiang Zhou , Si Liu , Pingping Zhu , Wei Shao . 氨基酸的衍生及手性气相色谱分离创新实验. University Chemistry, 2025, 40(6): 286-295. doi: 10.12461/PKU.DXHX202407059
14. [14]
  Shuai Yuan , Yaofeng Yuan . Academician Chengye Yuan and Organic Phosphorus Chemistry. University Chemistry, 2025, 40(7): 393-400. doi: 10.12461/PKU.DXHX202409123
15. [15]
  Ke Qiu , Fengmei Wang , Mochou Liao , Kerun Zhu , Jiawei Chen , Wei Zhang , Yongyao Xia , Xiaoli Dong , Fei Wang . A Fumed SiO₂-based Composite Hydrogel Polymer Electrolyte for Near-Neutral Zinc-Air Batteries. Acta Physico-Chimica Sinica, 2024, 40(3): 2304036-0. doi: 10.3866/PKU.WHXB202304036
16. [16]
  Xiaohang JIN , Qi LIU , Jianping LANG . Room‑temperature solid‑state synthesis, structure, and third‑order nonlinear optical properties of phosphine‑ligand‑protected silver thiolate clusters. Chinese Journal of Inorganic Chemistry, 2025, 41(8): 1505-1512. doi: 10.11862/CJIC.20250125
17. [17]
  Zhanxiang Liu , Chengshan Yuan , Jie Han , Shuanglian Cai , Qihan Zhang , Lin Wu , Yuan Zheng , Xingwen Sun , Qingwen Liu , Ying Xiong , Guangao Yu , Xin Du , Houjin Li , Jianrong Zhang , Shuyong Zhang . Recommendations for Basic Operations and Standards for Organic Chemical Extraction and Washing Experiments. University Chemistry, 2025, 40(5): 55-65. doi: 10.12461/PKU.DXHX202410039
18. [18]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
19. [19]
  Yajie Li , Bin Chen , Yiping Wang , Hui Xing , Wei Zhao , Geng Zhang , Siqi Shi . Inhibiting Dendrite Growth by Customizing Electrolyte or Separator to Achieve Anisotropic Lithium-Ion Transport: A Phase-Field Study. Acta Physico-Chimica Sinica, 2024, 40(3): 2305053-0. doi: 10.3866/PKU.WHXB202305053
20. [20]
  Fan Wu , Wenchang Tian , Jin Liu , Qiuting Zhang , YanHui Zhong , Zian Lin . Core-Shell Structured Covalent Organic Framework-Coated Silica Microspheres as Mixed-Mode Stationary Phase for High Performance Liquid Chromatography. University Chemistry, 2024, 39(11): 319-326. doi: 10.12461/PKU.DXHX202403031

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(605)
HTML views(34)

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142