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

Detection of 9 β-agonists Illegally Added in Florfenicol Solid Preparation by UPLC-MS/MS

关键词:  β-受体激动剂、氟苯尼考固体制剂、非法添加、超高效液相色谱-串联质谱

Key words:  β-agonists  Florfenicol solid preparation  Illegal additives  UPLC-MS/MS

摘要:

本方法经0.1M盐酸-甲醇(1:1)提取,0.1%的甲酸溶液稀释,BEH C₁₈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0.99；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。

Abstract:

A detection method for β-agonists illegally added such as clenbuterol、hydroxymethyl、salbutamol、cimaterol、cimbuterol、tulobuterol、mabuterol、terbutaline and clorprenaline in Florfenicol solid preparation was established, Sample was extracted by 0.1M Hydrochloric acid-Methanol (1:1,V/V) and was diluted by 01.% formic acid. The separation of β-agonists was performed with BEH C18 column and was analyzed by Ms/MS. The calibration curves were good linear between serial concentrations, the correlation coefficient r₂＞0.99. The limits of detection of 9 β-agonists in Florfenicol solid preparation were 500mg/kg, and the quantification was 1000mg/kg.The average recoveries were in the ranged of 90.8 %～103.4 %. The intra- and inter-batch variation corfficinets wer both less than 10%. So, this method was rapid, simple and qualitative accurately.