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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
周炜,陈慧华
0
(浙江省兽药监察所)
摘要:
建立了同时测定动物尿液中23种?-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?-受体激动剂的定量下限(LOQ)为0. 1~1.0 μg/L。用猪、牛及羊尿样为研究对象,考察方法的准确度及精密度。23种?-受体激动剂在0.5 μg/L、1.0 μg/L和10 μg/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?-受体激动剂类药物的残留检测任务。
关键词:  动物尿液  b-受体激动剂  高效液相色谱-串联质谱法
DOI:
投稿时间:2013-05-13修订日期:2013-08-19
基金项目:公益性行业专项(201203023-4)
Determination of 23 β-agonists in Animal Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry
(Zhejiang Provincial Supervisory Institute of Veterinary Drug)
Abstract:
A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was established for the determination of twenty-three 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 (MRM). The limits of quantitation (LOQs) 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.
Key words:  animal urine  β-agonist  LC-MS/MS

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