通过式固相萃取/超高效液相色谱-串联质谱法快速测定鸡蛋中的8种兽药残留  

Determination of Eight Veterinary Drugs in Eggs by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with a Through-type Solid-phase Extraction

作　　者：金晓峰 焦仁刚 赵贵 栾庆祥 黄鑫 周泽晓 王庆红 孙真峥 谢丽丽 郭靖 王关吉 汤翠 赵赞伟 JIN Xiaofeng;JIAO Rengang;ZHAO Gui;LUAN Qingxiang;HUANG Xin;ZHOU Zexiao;WANG Qinghong;SUN Zhenzheng;XIE Lili;GUO Jin;WANG Guanji;TANG Cui;ZHAO Zanwei(Guizhou Provincial Veterinary Drug and Feed Supervision Institute,Guiyang 550003;Tongren City Veterinary DrugSupervision Institute,Tongren 554300;Liupanshui City Veterinary Drug and Feed Supervision Institute,Liupanshui 553001;Zunyi City Veterinary Drug and Feed Supervision Institute,Zunyi 563000)

机构地区：[1]贵州省兽药饲料检测所,贵州贵阳550003 [2]铜仁市兽药监察所,贵州铜仁554300 [3]六盘水市兽药饲料监察所,贵州六盘水553001 [4]遵义市兽药饲料监测站,贵州遵义563000

出　　处：《分析科学学报》2020年第6期906-911,共6页Journal of Analytical Science

基　　金：贵州省科技计划(黔科合支撑[2019]2318号);贵州省农业农村厅科技项目(No.GZ2020JQFX0101)。

摘　　要：建立了通过式固相萃取,结合超高效液相色谱-串联质谱法(UPLC/MS/MS)快速测定鸡蛋中硝基咪唑类(甲硝唑、地美硝唑)、酰胺醇类(氯霉素、氟苯尼考、甲砜霉素)、尼卡巴嗪、金刚烷胺和灭蝇胺8种兽药残留量的方法。样品采用80%乙腈(0.1%甲酸酸化)提取,PRiME HLB固相萃取净化,UPLC/MS/MS测定残留量。结果表明,8种化合物浓度在1.00~500.0 ng/mL范围内线性关系良好,相关系数(R2)大于0.997,检出限为0.3~5.0μg/kg,定量限为1.0~10.0μg/kg,在3个加标水平下的回收率为64.5%~109.3%,批内相对标准偏差为1.6%~11.8%,批间相对标准偏差为2.1%~13.5%。该方法快速、灵敏、准确、稳定,符合兽药残留检测方法性能要求,可实现鸡蛋中甲硝唑、地美硝唑、氯霉素、氟苯尼考、甲砜霉素、尼卡巴嗪、金刚烷胺和灭蝇胺的同时快速测定。The pretreatment method of through-type solid-phase extraction was improved to be coupled with ultra performance liquid chromatography tandem mass spectrometry for detection of multiple residues of 8 veterinary drugs in eggs.The samples were extracted with 80% acetonitrile(formic acid acidification),and the supernatant was purified by PRiME HLB solid phase extraction,and then determined by UPLC-MS/MS.The results showed that 8 veterinary drugs had good linear relationship within the concentration range of 1.00-500.0 ng/mL(R^2≥0.997),and the LOD was within the range of 0.3-5.0 μg/kg,the LOQ was within the range of 1.0-10.0 μg/kg.The recovery of eight analytes at three concentration levels(LOQ,5 times of LOQ,10 times of LOQ) were within the range of 64.5%-109.3%,and the intra-day RSD was within the range of 1.6%-11.8%,the inter-day RSD was within the range of 2.1%-13.5%,respectively.This method is accurate,rapid,sensitive and stable,meets the requirement for the rapid determination of Metronidazole,Demenidazole,Chloramphenicol,Florfenicol,Thiamphenicol,Nicarbazine,Amantadine and Cyromazine in eggs.

关 键 词：通过式固相萃取 超高效液相色谱串联质谱 兽药残留 鸡蛋 

分 类 号：O657.63[理学—分析化学]