QuEChERS-HPLC-MS/MS测定动物源食品中环己烯酮类除草剂残留量

为建立动物源食品中环己烯酮类除草剂残留量同时测定的液相色谱- 质谱/ 质谱方法，将试样中残留的环己烯酮类除草剂用酸性乙腈高速匀浆提取，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，用液相色谱- 质谱/ 质谱仪检测和确证，外标法定量。结果表明：环己烯酮类除草剂的质量浓度在0.0025～0.1000μg/mL 范围内时，线性关系良好，8 种环己烯酮类除草剂的相关系数为0.9973～0.9996；在0.005～0.050mg/kg 范围内，样品平均加标回收率在75.68%～106.80% 之间，相对标准偏差为6.65%～11.04%；8 种环己烯酮类除草剂的最低检出限均为0.005mg/kg。

Determination of Cyclohexanediones Herbicide Residues in Foodstuffs of Animal Origin by QuEChERS-HPLC-MS/MS

A HPLC-MS/MS method based on QuEChERS extraction has been developed for determining cyclohexanediones herbicide residues in foodstuffs of animal origin. Cyclohexanediones herbicide residues in samples were extracted with acidic acetonitrile under the assistance of high-speed homogenization. The extract was cleaned up with N-propyl ethylenediamine (PSA), octadecylsilane (ODS) and graphitized carbon black prior to HPLC-MS/MS analysis. The calibration curves of 8 cyclohexanedione compounds developed all exhibited good linearity over a concentration range from 0.0025 to 0.1000 μg/mL, with a correlation coefficient ranging from 0.9973 to 0.9996. Average recoveries for the analytes in pork spiked at 0.005, 0.010 mg/kg and 0.050 mg/kg were between 75.68% and 106.80%, with a relative standard deviation between 6.65% and 11.04%. The detection limit was 0.005 mg/kg for all of the analytes.