高效液相色谱-串联质谱法测定动物尿液中23种β-受体激动剂

Determination of 23 β- agonists in Animal Urine by High Performance Liquid Chromatography- Tandem Mass Spectrometry

建立了同时测定动物尿液中23种β-受体激动剂的高效液相色谱-串联质谱检测法。样品用2 mol/L盐酸酸解,经过SLS固相萃取柱净化、富集后,以甲醇和0.2%甲酸水溶液为流动相进行梯度洗脱,采用多反应监测模式进行定性和定量分析。23种β-受体激动剂的定量下限为0.1～1.0μg/L。用猪、牛及羊尿样为研究对象,23种β-受体激动剂在0.5、1.0和10μg/L三个水平下的平均回收率为68%～115%,批内相对标准偏差为0.5%～9.6%,批间相对标准偏差0.6%～14.1%。结果表明,该方法具有准确、简便、灵敏,重现性好等特点,能满足β-受体激动剂类药物的残留检测任务。

A high performance liquid chromatography - tandem mass spectrometry （ LC - MS/MS） method was established for the determination of 23 β - agonists in animal urine. The 2 mol/L hydrochloric acid was used to acidify the sample, and then the sample was purified and concentrated by an SLS SPE column. The separation of the β- agonists was performed on a HPLC system, which was using gradient elution with methanol and 0. 2% formic acid. Qualitative and quantitative analysis of the 23 β - agonists were carried out in multiple reactions monitoring mode. The limits of quantitation of 23 β - agonists were in the range of 0. 1 - 1.0 μg/L. The spiked swine, bovine and goat urine were used to investigate the exactitude and accuracy of this method. The results showed that when the concentrations of the 23 β - agonists were between 0. 5 and 10 μg/L, the average recoveries ranged from 68% to 115%, the CV for within -run assays and between -run assays were 0. 5% -9.6% and 0. 6% -14. 1%. The method was veracious, sample, sensitive and repeatable, and it was well suitable for the determination of β -agonists in animal urine.