固相萃取-气相色谱-串联质谱法测定大豆油中126种农药残留  

Determination of 126 pesticides residues in soybean oil by solid phase extraction-gas chromatography-tandem mass spectrometry

作　　者：汪春明 张洋[1] 王东斌 施鹏斐 杨波 WANG Chunming;ZHANG Yang;WANG Dongbin;SHI Pengfei;YANG Bo(Chinese Academy of Inspection and Quarantine Comprehensive Test Center,Beijing 100123,China)

机构地区：[1]中国检验检疫科学研究院综合检测中心,北京100123

出　　处：《农药学学报》2021年第2期405-413,共9页Chinese Journal of Pesticide Science

摘　　要：建立了同时测定大豆油中126种农药残留的检测方法。样品经乙腈饱和的正己烷溶解并初次除油后用正己烷饱和的乙腈萃取,于-5℃、20 000 r/min下离心5 min,Captiva EMR-Lipid固相萃取柱净化,乙酸乙酯复溶后采用气相色谱-质谱联用仪(GC-MS/MS)多反应监测(MRM)模式检测,外标法定量。结果表明:在0.003~0.2 mg/L范围内,126种农药的质量浓度与其对应的峰面积间线性关系良好,R2均大于0.995,在0.005、0.01和0.05 mg/kg 3个添加水平下,126种农药的回收率在60%~119%之间,其中122种农药的RSD低于20%,另外4种农药的RSD低于25%。该方法能够有效除去大豆油中甘油及亲脂性干扰物,方法灵敏度、准确度和精密度均符合农药残留检测的要求,为监测大豆油中农药残留含量、有效防范健康风险提供了一种高效、可靠的分析手段。A multi-residue analysis method was established for simultaneous determination of 126 pesticides in soybean oil using SPE-gas chromatography-tandem mass spectrometry(GC/MS/MS). The samples were degreased by n-hexane saturated with acetonitrile and extracted by n-hexane saturated acetonitrile under mechanical shaking. Then the extracts were centrifuged at -5 ℃ and 20 000 r/min for 5 min, and cleaned-up with Captiva EMR-Lipid solid phase extraction column. After being re-dissolved with ethyl acetate, the samples were detected using multiple reaction monitoring(MRM) on GCMS/MS system and quantified with external standard method using matrix matched calibration curves.The results showed that: in the range of 0.003-0.2 mg/L, good linear relationship were obtained between the concentrations of 126 pesticides and their corresponding peak areas, and the R2 was greater than 0.995. The recoveries of 126 pesticides ranged from 60% to 119% at the spiked levels of 0.005, 0.01 and 0.05 mg/kg. The RSDs were lower than 20% for 122 pesticides, and were lower than 25% for the other four pesticides. The method can effectively remove glycerolipid and some lipophilic interference from the soybean oil. The sensitivity, accuracy and precision of the method meet the requirements of pesticide residue detection. It provides an efficient and reliable analytical method for monitoring the level of pesticide residues in soybean oil and effectively preventing the health risks.

关 键 词：固相萃取 气相色谱-串联质谱 多反应监测(MRM) 大豆油 农药多残留 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]