| 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HPLC-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。 |
| 关键词: 诺氟沙星 盐酸小檗碱 盐酸氯苯胍 水产品 液质联用 |
| DOI： |
| 投稿时间：2014-06-17修订日期：2014-08-04 |
| 基金项目: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) |
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| Determination of Norfloxacin, Berberine Hydrochloride and Robenidine Hydrochloride Residues in Aquatic Products by High Performance Liquid Chromatography-mass Spectrometry（HPLC-MS/MS） |
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| (Guangdong Ocean University,Fisheries College,Zhanjiang) |
| Abstract: |
| 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. |
| Key words: norfloxacin berberine hydrochloride robenidine hydrochloride aquatic products HPLC-MS/MS |
