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建立了大豆中虫酰肼残留量测定的高效液相色谱-电喷雾串联质谱(HPLC-ESI-MS/MS)检测方法。样品中残留的虫酰肼用酸性乙腈匀浆提取,提取液经N-丙基乙二胺(PSA)、十八烷基硅烷(ODS)和石墨化炭黑净化,用反相高效液相色谱柱分离后进行质谱分析检测和确证,外标法定量。虫酰肼的浓度在0.0004μg/mL~0.5000μg/mL范围内时,线性关系良好,虫酰肼相关系数(r2)为0.9933。在0.001mg/kg~0.500mg/kg浓度范围内,样品平均加标回收率在82.00%~107.02%之间,相对标准偏差为5.22%~8.71%。最低检出限为0.001mg/kg。
A high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS / MS) method for the determination of tebufenozide in soybean was established. The residual tebufenozide in the sample was extracted with acidic acetonitrile and the extract was purified with N-propyl ethylenediamine (PSA), octadecylsilane (ODS) and graphitized carbon black. The residue was purified by reversed-phase high performance liquid chromatography Column separation mass spectrometry detection and confirmation, external standard method. The linear relationship was good when the concentration of tebufenozide was in the range of 0.0004μg / mL to 0.5000μg / mL, and the correlation coefficient (r2) of tebufenozide was 0.9933. In the range of 0.001mg / kg ~ 0.500mg / kg, the average recoveries of samples ranged from 82.00% to 107.02% with relative standard deviations of 5.22% ~ 8.71%. The minimum detection limit of 0.001mg / kg.