Takatori Satoshi, Yamamoto Haruna, Fukui Naoki, Yamaguchi Satoko, Kitagawa Yoko, Kakimoto You, Osakada Masakazu, Okihashi Masahiro, Kajimura Keiji, Obana Hirotaka
Osaka Prefectural Institute of Public Health, 1-3-69 Nakamichi, Higashinari-ku, Osaka 537-0025, Japan.
Shokuhin Eiseigaku Zasshi. 2013;54(3):237-49. doi: 10.3358/shokueishi.54.237.
A validation study was conducted on a rapid multiresidue method for determination of pesticide residues in vegetables and fruits by LC-MS/MS. Pesticide residues in the vegetables or fruits were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride in the presence of citrate salts for buffering. The extract was purified with a double-layered cartridge column (graphite carbon black/primary secondary amine silica gel; GCB/PSA). For citrus fruits a purification step with a C18 column was added (this column was connected to the GCB/PSA column). After removal of the solvent, the extract was resolved in methanol/water and analyzed by means of LC-MS/MS. The method was validated according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan; recovery tests were performed on 8 kinds of vegetables and fruits [cabbage, cucumber, Japanese radish, onion, potato, spinach, Amanatsumikan (a citrus fruit) and apple] by fortification of 161 pesticide residues at the concentrations 0.01 and 0.05 μg/g (each concentration of pesticide residue was extracted from 2 samples on 5 separate days). The trueness of the method for 127 pesticides in all 8 commodities was 70-120% with satisfactory repeatability and within-run reproducibility. This method is concluded to be applicable for determination of pesticide residues in vegetables and fruits.
采用液相色谱-串联质谱法（LC-MS/MS）对一种快速多残留方法测定蔬菜和水果中农药残留进行了验证研究。蔬菜或水果中的农药残留采用匀浆机在一次性试管中用乙腈提取，然后在柠檬酸盐存在下用无水硫酸镁和氯化钠进行盐析以缓冲。提取物用双层柱（石墨化炭黑/伯仲胺硅胶；GCB/PSA）净化。对于柑橘类水果，增加了一个用C18柱的净化步骤（该柱与GCB/PSA柱相连）。去除溶剂后，提取物用甲醇/水溶解并通过LC-MS/MS进行分析。该方法根据日本厚生劳动省的方法验证指南进行验证；通过在0.01和0.05μg/g浓度下添加161种农药残留对8种蔬菜和水果[卷心菜、黄瓜、白萝卜、洋葱、土豆、菠菜、甘夏蜜柑（一种柑橘类水果）和苹果]进行回收率测试（每种农药残留浓度从5个不同日期的2个样品中提取）。该方法对所有8种商品中127种农药的准确度为70-120%，具有令人满意的重复性和批内重现性。得出该方法适用于测定蔬菜和水果中农药残留的结论。
