HPLC-MS/MS法同时测定水产品中的诺氟沙星、盐酸小檗碱、盐酸氯苯胍残留  

Determination of Norfloxacin,Berberine Hydrochloride and Robenidine Hydrochloride Residues in Aquatic Products by High Performance Liquid Chromatography-mass Spectrometry(HPLC-MS/MS)

作　　者：汤菊芬[1,2] 蔡佳[1,2] 廖建萌 王蓓[1,2] 秦青英[1,2] 黄月雄 简纪常[1,2] 

机构地区：[1]广东海洋大学水产学院,广东湛江524088 [2]广东省水产经济动物病原生物学及流行病学重点实验室,广东湛江524088 [3]广东省湛江市质量计量监督检测所,广东湛江524022

出　　处：《中国兽药杂志》2014年第8期55-60,共6页Chinese Journal of Veterinary Drug

基　　金：广东省科技计划(农业攻关)项目(2012B020308010);农业部公益性行业专项(20120385)

摘　　要：建立了一种同时测定水产品中诺氟沙星、盐酸小檗碱和盐酸氯苯胍残留量的HP LC-MS/MS法。样品经1％甲酸甲醇提取，正己烷脱脂，冷冻、离心后，用高效液相色谱-串联质谱仪，选择反应监测（ SRM）、正离子模式进行定性和定量分析。结果表明：诺氟沙星、盐酸小檗碱和盐酸氯苯胍在1～100 ng/mL范围内线性关系良好，线性相关系数≥0．9996，检出限为1 ng/g。诺氟沙星、盐酸小檗碱、盐酸氯苯胍在5、50和100 ng/g三个添加水平下，三种水产品肌肉的平均加标回收率在79．83％～104．06％之间，相对标准偏差在2．97％～9．15％之间。本方法重现性好，灵敏度高，能够满足水产品中诺氟沙星、盐酸小檗碱和盐酸氯苯胍的残留检测和药代动力学的研究需要。An analytical HPLC-MS/MS method was established for determination of norfloxacin （ NFLX ） , berberine hydrochloride（ BBH） and robenidine hydrochloride（ ROBH） residues in aquatic products. The samples were extracted with methanoic acid-methanol （1 ∶ 99,V/V）, then defatted with n-hexane. The treated samples were analyzed by HPLC-MS/MS after freezed and centrifuged. The analysis was performed with selected reaction monitoring （ SRM） in positive ion mode. The results indicated good linearities in the concentration range from 1~100 ng/mL for NFLX, BBH and ROBH, the correlation coefficient and the detection limit were 0. 9997 and 1 ng/g, respectively. While the spiked contents of NFLX, BBH and ROBH standard at 5, 50, 100 ng/g, the recoveries and relative standard deviations （ RSD ） were in range of 79. 83%~104. 06% and 2. 97%~9. 15%, respectively. This method was suitable for detection and pharmacokinetics study of NFLX, BBH and ROBH residues in aquatic products.

关 键 词：诺氟沙星 盐酸小檗碱 盐酸氯苯胍 水产品 液质联用 

分 类 号：S859.84[农业科学—临床兽医学]