Saito-Shida Shizuka, Nemoto Satoru, Matsuda Rieko
National Institute of Health Sciences.
Shokuhin Eiseigaku Zasshi. 2014;55(3):142-51. doi: 10.3358/shokueishi.55.142.
A multiresidue method for analyzing pesticides in vegetables and fruits by supercritical fluid extraction (SFE) and LC-MS/MS was developed. The sample preparation and SFE parameters were optimized for extracting LC-amenable polar and medium-polarity pesticides. High recoveries were achieved for most of the tested pesticides by extracting a 1 : 1 : 1 sample-Celite-anhydrous magnesium sulfate mixture with supercritical carbon dioxide at 16.4 MPa at 40℃ for 30 min with methanol added as a modifier. The recoveries of 117 pesticides fortified with 0.01 mg/kg of each pesticide were 70-120%, and the relative standard deviations were less than 25% for 112 pesticides in tomato and 103 pesticides in cucumber. No significant differences were observed in the residue concentrations determined in real samples by the SFE method and the liquid extraction method (the modified Japanese official method). Higher recoveries of polar pesticides, such as acephate and methamidophos, were achieved by the developed SFE method than by the liquid extraction method.
建立了一种采用超临界流体萃取（SFE）和液相色谱 - 串联质谱（LC-MS/MS）分析蔬菜水果中农药的多残留方法。针对可用于液相色谱分析的极性和中等极性农药，对样品制备和SFE参数进行了优化。通过在40℃、16.4 MPa条件下，用超临界二氧化碳萃取1:1:1的样品 - 硅藻土 - 无水硫酸镁混合物，并添加甲醇作为改性剂30分钟，大多数被测农药获得了高回收率。添加浓度为0.01 mg/kg的117种农药在番茄中的回收率为70 - 120%，112种农药的相对标准偏差小于25%；在黄瓜中，103种农药的回收率为70 - 120%，相对标准偏差小于25%。通过SFE方法和液体萃取法（改进的日本官方方法）测定实际样品中的残留浓度，未观察到显著差异。与液体萃取法相比，所建立的SFE方法对乙酰甲胺磷和甲胺磷等极性农药具有更高的回收率。
