超高效液相色谱-质谱串联法测定牦牛肉中11种喹诺酮类药物残留  

Determination of 11 quinolone residues in yak meat by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：龙启萍[1] 曹海兰[1] 吕东晋[1] 龙启福[2] 刘双德[1] LONG Qiping;CAO Hailan;LV Dongjin;LONG Qifu;LIU Shuangde(Qinghai Province Center for Disease Control and Prevention, Xining 810007, China)

机构地区：[1]青海省疾病预防控制中心,西宁810007 [2]青海大学医学院

出　　处：《医学动物防制》2018年第6期570-573,共4页Journal of Medical Pest Control

基　　金：青海省科技项目(2015-ZJ-Y23)

摘　　要：目的建立牦牛肉中11种喹诺酮类农药残留的超高效液相色谱-串联质谱监测分析方法。方法样品经20ml,0.1 mol/L EDTA-Mcllvaine缓冲液(pH=4.0)匀浆后采用2.5 ml酸性乙腈(含0.2%甲酸)沉淀蛋白,上清液经HLB固相萃取柱净化,用Thermo C18小柱(100 mm×2.1 mm,2.2μm),以甲醇-乙腈溶液(40+60)-0.2%甲酸水溶液为流动相、多反应监测(MRM)正离子扫描方式进行质谱检测,内标法定量。结果添加浓度在1.5~10.0μg/kg时,11种喹诺酮药物在牦牛肉中的平均回收率为84.2%~97.7%,RSD为5.2%~12.1%,在2.5~100.0μg/L范围内线性良好,11种喹诺酮药物的相关系数r≥0.995。结论该方法简单、灵敏、特异性强,适用于牦牛肉中喹诺酮类药物多残留的检测。Objective Establishment of super-performance liquid chromatography-tandem mass spectrometry monitoring method for determination of 11 quinolone pesticide residues in yak meat. Methods The samples were homogenized with 20 ml of0. 1 M EDTA-Mcllvaine buffer(pH = 4. 0） and the proteins were precipitated with 2. 5 ml of acidic acetonitrile(containing0. 2% formic acid）. The supernatant was purified by HLB SPE using Thermo C18(100 mm × 2. 1 mm,2. 2 μm） with a mobile phase of methanol-acetonitrile solution(40 ＋ 60）-0. 2% formic acid as mobile phase and multiple reaction monitoring(MRM）. Results The average recoveries of 11 quinolones in yak meat ranged from 84. 2% to 97. 7% with a RSD of 5. 2% to12. 1% at concentrations ranging from 1. 5 to 10. 0 μg/kg,with good linearity in the range of 2. 5 to 100. 0 μg/L,the correlation coefficients of 11 quinolone drugs were r≥0. 995. Conclusion The method is simple,sensitive and specific and is suitable for the detection of quinolone residues in yak meat.

关 键 词：超高效液相色谱-串联质谱 喹诺酮类 全自动固相萃取仪 牦牛肉 

分 类 号：R155.55[医药卫生—营养与食品卫生学]