气相色谱-质谱法测定动物肌肉中314种农药残留

Analysis of 314 Pesticide Residue in Animal Muscles by Solid Phase Extraction- gas Chromatography- mass Spectrometry

建立固相萃取-气相色谱-质谱（SPE-GC-MS）法测定动物肌肉中314种农药残留的分析方法。样品用乙腈-水溶液均质提取，加盐后继续均质，离心后取部分乙腈提取液过Envi-18和LC-NH2串联柱净化后供气相色谱-质谱仪分析。采用外标定量法，选择离子扫描方式，对前处理条件和仪器参数进行优化，在最优试验条件下进行测试，检出限（S/N≥10）为0.01-0.05 mg/kg，相对标准偏差为4.6%-15.1%，回收率为58.7%-161.2%，其中回收率为70%-120%的目标物占81.2%。

A solid phase extraction - gas chromatography - mass spectrometry analysis method for variety of pesticide residue in animal muscles has been developed. The samples are extracted homogeneously in acetonitrile - water solution firstly, and continue to homogenize after adding salt into the above solution. And then centrifugation, the clear supernatant is purified （Envi-18 and LC-NH2 column） to be ready for GC-MS analysis which is performed by using selected ion monitoring （SIM） mode. The pretreatment conditions and instrument parameters are optimized in the study, and all factors are discussed deeply. Under optimal conditions, the detection limits of the proposed method （S/N≥10） are found in the ranges of 0.01-0.05 mg/kg, the recoveries are in the ranges of 58.7%-161.2% which contains 81.2% of projects＆#39; recoveries being in the ranges of 70%-120%, and the relative standard deviations are 4.6%-15.1%.