超高效液相色谱-串联质谱法检测氟苯尼考固体制剂中9种β-受体激动剂

摘要

采用0．1 mol／L盐酸-甲醇（1∶1）提取，0．1％甲酸溶液稀释，BEHC18色谱柱分离，串联质谱分析，对氟苯尼考固体制剂中克伦特罗、莱克多巴胺、沙丁胺醇、西马特罗、西布特罗、妥布特罗、马布特罗、特布他林、氯丙那林等9种β-受体激动剂非法添加物进行检测分析。9种β-受体激动剂在系列浓度范围内呈现良好线性关系，相关系数r2均大于0．990；9种药物在氟苯尼考固体制剂中的检出限为500 mg／kg，定量限为1000 mg／kg，回收率为90．8％～103．4％，批内、批间相对标准偏差均小于10％。结果表明，该方法简便快捷、定性准确，适用于该类药物在氟苯尼考固体制剂中的检测。%A detection method for β-agonists illegally added such as clenbuterol, ractopamine, salbutamol, cimaterol, cimbuterol, tulobuterol, mabuterol, terbutaline and clorprenaline in florfenicol solid preparation was established.Sample was extracted by 0.1 mol/L hydrochloric acid-methanol (1 ∶ 1,V/V) and was diluted by 0.1% formic acid. The separation of β-agonists was performed with BEHC18 column and was analyzed by MS/MS. The calibration curves were good linear between serial concentrations, the correlation coefficient r2>0. 990. The limits of detection of 9 β-agonists in florfenicol solid preparation were 500 mg/kg, and the quantification was 1000 mg/kg.The average recoveries were in the ranged of 90.8%~103.4%. The intra- and inter-batch variation corfficinets were both less than 10%. So this method was rapid, simple and qualitative accurately.