QuEChERS-气相色谱-三重四极杆串联质谱法高通量测定畜肉中16种镇静剂药物残留

High-throughput detection of 16 sedative drug residues in livestock meat using QuEChERS-GC-MS/MS

[目的]本文旨在构建一种QuEChERS结合气相色谱-三重四极杆串联质谱法高通量测定猪、牛、羊等畜肉中16种镇静剂类药物残留的方法。[方法]畜肉样品经乙腈提取,柠檬酸缓冲体系盐包盐析脱水,无水硫酸钠、N-丙基乙二胺吸附剂净化,再经TR-PesticideⅡ毛细管柱分离,在多反应监测模式下测定镇静剂类药物残留,外标法定量。[结果]16种镇静剂药物在1~200 ng·mL^(-1)的浓度范围内线性良好(R^(2)≥0.9928),检出限为0.01~0.30μg·kg^(-1),定量限为0.10~1.00μg·kg^(-1)。在0.10~10.00μg·kg^(-1)的加标水平下,回收率为64.83%~112.04%,批内相对标准偏差为1.45%~8.96%,批间相对标准偏差为4.48%~14.88%。[结论]该方法操作简便,灵敏度和精密度高,分析时间短且重现性好,可满足畜肉中多种镇静剂类药物残留的快速检测。

[Objectives]The purpose of this paper was to develop a method of the high throughput determination of 16 sedative drug residues in pig,cattle and sheep meat by QuEChERS(quick,easy,cheap,effective,rugged,safe)combined with gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).[Methods]The samples of livestock meat were extracted by acetonitrile.The extracts were dehydrated by salt-packed salting in a citric acid buffer system,purified by Na 2SO 4 and primary secondary amine(PSA)sorbent,separated by a TR-PesticideⅡcapillary column.The sedative drug residues were determined in multiple reaction monitoring mode and quantified by external standard method.[Results]The 16 sedative drugs showed good linearity in the concentration range of 1-200 ng·mL^(-1)(R^(2)≥0.9928).The limit of detection was 0.01-0.30μg·kg^(-1)and the limit of quantification was 0.10-1.00μg·kg^(-1).At the spiked levels of 0.10-10.00μg·kg^(-1),the recovery ranged from 64.83%to 112.04%,the intra-batch relative standard deviation(RSD)was 1.45%-8.96%,and the inter-batch RSD was 4.48%-14.88%.[Conclusions]The method was simple with high sensitivity and precision,short analysis time and good reproducibility.It could meet the need of rapid detection of various sedative drug residues in livestock meat.