摘要
建立了通过型SPE柱Oasis PRiME HLB固相萃取柱净化-高效液相色谱-串联质谱法,同时测定动物肌肉、动物尿液中9种β-受体激动剂类药物残留含量。对于肌肉样品,加入pH 5.20.2M乙酸铵溶液和β-葡萄糖醛苷酶振荡16 h,在样品中添加乙腈(含0.2%甲酸)、氯化钠,震荡后离心取上清液过固相萃取小柱,氮吹近干,定容后上机检测。对于尿液样品,省去酶解步骤,直接用乙腈溶液提取后净化,上机检测。该方法的前处理过程较为简便高效,加标回收率为91%~100%,相对标准偏差为2%~6%。9种β-受体激动剂药物的检测限均低于0.5μg/kg,适应于日常样品快速筛查的要求。
The Oasis PRiME HLB SPE purification method was established for the analysis of 9β-adrenoceptor agonists residues in animal derived samples by using HPLC-MS-MS.For animal muscle samples detection,pH=5.20.2 mol/L ammonium acetate solution andβ-Glucuronidase were added and shaken for 16hrs.Then acetonitrile(including 0.2%formic acid),sodium chloride were added.After oscillation and then centrifugation,liquid supernatant was nearly dried by nitrogen blow,and then checked after the volume was regulated.For urine samples,the enzymatic hydrolysis step was omitted,before detection,extraction with acetonitrile solution and purification was implemented.The pretreatment process of this method is relatively simple and efficient,with a standard recovery rate of 91%~100%and a relative standard deviation of 2%~6%.The detection limits of the 9β-adrenoceptor agonist drugs were all below 0.5μg/kg,meeting the requirements of the rapid screening of daily samples.
作者
邓艳芹
汪坤乾
廖金兰
吕建平
倪杨帆
DENG Yanqin;WANG Kunqian;LIAO Jinlan;LYU Jianping;NI Yangfan(Wuhan Agricultural Inspection Center,Wuhan 430016,Hubei,China)
出处
《咸阳师范学院学报》
2022年第4期25-29,共5页
Journal of Xianyang Normal University
