摘要
建立了膏方中药制剂中甲硝唑、地美硝唑、洛硝哒唑、替硝唑、洛美沙星、培氟沙星、氧氟沙星、诺氟沙星、氨苯砜和氯霉素等10种兽药残留的HPLC-MS/MS测定方法。样品经Mcllvaine缓冲溶液(pH4.0)稀释,以乙腈作为提取溶剂,选择900 mg无水MgSO4、50 mg N-丙基乙二胺、50 mg十八烷基键合硅胶的组合为吸附剂去除膏方中药制剂中的糖类、多酚类、黄酮类等干扰物。试样溶液经HPLC-MS/MS测定,内标法定量。目标化合物在相应的浓度范围内线性关系良好,相关系数均大于0.9996,方法检出限为0.04~0.32μg/kg,定量限为0.1~0.8μg/kg。目标化合物的平均回收率为60.4%~114.0%,相对标准偏差范围为1.9%~9.9%。
A method for the determination of 10 kinds of veterinary drug residues in traditional Chinese medicine soft extract was developed,which was suitable for the determination of metronidazole,demenidazole,lonidazole,tinidazole,lomefloxacin,pefloxacin,ofloxacin,norfloxacin,dapsone and chloramphenicol.Target compounds were extracted by acetonitrile after the dissolution of the sample with Mcllvaine buffer solution(pH 4.0).900 mg of anhydrous magnesium sulfate,50 mg of N-Propylethylenediamine and 50 mg of octadecylsilane were selected as adsorbents to remove the interferences such as sugars,polyphenols and flavonoids.Target compounds were determined by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)and quantified by internal standard method.The linear relationships of the target compounds were good in the corresponding concentration ranges,and the correlation coefficients were greater than 0.9996.The detection limits were 0.04-0.32μg/kg,and the limits of quantification were 0.1-0.8μg/kg.The average recoveries of the target compounds ranged from 60.4%to 114.0%,with the relative standard deviations in the range from1.9%to 9.9%.
作者
温家欣
陈俏
曹雅静
何嘉雯
赖宇红
WEN Jiaxin;CHEN Qiao;CAO Yajing;HE Jiawen;LAI Yuhong(Guangdong Institute for Drug Control,Guangzhou 510663)
出处
《分析试验室》
CAS
CSCD
北大核心
2021年第5期541-546,共6页
Chinese Journal of Analysis Laboratory
基金
国家药品监督管理局药品快速检验技术重点实验室项目(国药监科外函[2019]82号-24)资助。
