摘要
建立了畜禽粪便中3种β-受体激动剂药物残留的超高压液相色谱-串联四极杆质谱联用仪测定方法。样品酶解后经高氯酸溶液净化,调节p H值至碱性,乙酸乙酯提取,净化浓缩后以流动相定容,用超高压液相色谱-质谱联用仪检测,内标法定量。3种β-受体激动剂在0.5~20.0μg/L范围内线性关系良好,相关系数均大于0.998。畜禽粪便中3种β-受体激动剂的加标回收率为80.3%~110.2%,相对标准偏差为3.0%~7.7%,检出限（S/N=3）为0.04~0.07μg/kg。
A method for the simultaneous determination of 3β-agonists in animal manure was studied by ultra high performance liquid chromatography coupled with electrospray ionization triple - quadrup- le tandem mass spectrometry（ UPLC -ESI MS/MS）. The drugs were cleaned up with perehloric acid solution after enzymolysis and adjusting pH to alkaline. The purified analyte was extracted with ethyl acetate. The extract was evaporated to dryness under nitrogen, and reconstituted in mobile phase so- lution. The target compounds were confirmed and quantified by UPLC - ESI MS/MS with the internal standard method. Under the optimal conditions, the calibration curves of 3β-agonists showed good linearities in the range of 0. 5 - 20. 0 μg/L with correlation coefficients more than 0. 998. The aver- age recoveries of 3 β-agonists were in the rarLge of 80. 3% - 110. 2% , and the relative standard deviations （RSDs） were 3. 0% - 7. 7%. The limits of detection （S/N = 3 ） ranged from 0. 04 μg/kg to 0. 07 μg/kg.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第1期74-78,共5页
Journal of Instrumental Analysis
基金
北京市农委基金项目(PXM2014 036240 000012)
关键词
超高压液相色谱-串联四极杆质谱联用仪
畜禽粪便
β-受体激动剂
内标法
ultra high performance liquid chromatography coupled with electrospray ionization triple-quadruple tandem mass spectrometry（ UPLC -ESI MS/MS）
animal manure
β-agonists
internal standard method
