Lee Sung Joong, Park Semin, Choi Jin Young, Shim Jae-Han, Shin Eun-Ho, Choi Jeong-Heui, Kim Soo Taek, Abd El-Aty A M, Jin Jong Sung, Bae Dong Won, Shin Sung Chul
Department of Chemistry, Gyeongsang National University, Jinju, Republic of Korea.
Biomed Chromatogr. 2009 Jul;23(7):719-31. doi: 10.1002/bmc.1176.
It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean-up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB-C(18) column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100gamma(ij) (%). A high matrix effect (<-30%) was detected for the seven polar pesticides, namely thiamethoxam, clothianidin, acetamiprid, aldicarb, thiacloprid, pirimicarb and methabenzthiazuron. The limits of detection were in the range of 0.1-8.1 microg/kg, indicating a good sensitivity. Most of the recoveries ranged from 70 to 131% with RSDs <or= 20%. The current method allowed rapid quantitation and identification of low pesticide levels in the cooked vegetable samples. Of the screened pesticide residues, only fluquinconazole and dimethomorph below the maximum residue levels established by the KFDA were detected in onion and cucumber samples.
对于具有可水解官能团的农药残留，最好在烹饪后进行分析，因为它们的结构在煮沸和/或加热过程中容易降解。本文描述了一种液相色谱-串联质谱（LC-MS/MS）方法，用于定量测定韩国广泛消费的五种典型蔬菜中44种具有可水解官能团的农药残留。样品净化按照韩国食品药品管理局（KFDA）制定的食品法典第83号方法进行。由于峰分离效果最佳，选择了Zorbox XDB-C(18)柱进行分析。LC流动相由水和5 mM甲酸甲醇铵组成，每次运行时峰形对称良好。串联质谱（MS/MS）实验在ESI正模式和多反应监测模式下进行。传统的基质效应被修改为更全面的形式100γ(ij)（%）。七种极性农药，即噻虫嗪、氯噻啉、啶虫脒、涕灭威、噻虫啉、抗蚜威和甲基苯噻隆，检测到高基质效应（<-30%）。检测限在0.1-8.1 μg/kg范围内，表明灵敏度良好。大多数回收率在70%至131%之间，相对标准偏差（RSDs）≤20%。该方法能够快速定量和鉴定烹饪蔬菜样品中的低农药含量。在筛选的农药残留中，仅在洋葱和黄瓜样品中检测到低于KFDA规定的最大残留限量的氟喹唑和烯酰吗啉。
