摘要
建立了液相色谱-串联质谱测定猪尿液中异丙喘宁、氯丙那林、西马特罗、特布他林、妥布特罗、西布特罗、沙丁胺醇、齐帕特罗、克伦特罗、莱克多巴胺、非诺特罗、马布特罗、溴代克伦特罗、马贲特罗、苯乙醇胺A、溴布特罗16种β受体激动剂的全自动分析方法。样品于37℃过夜酶解后,经阳离子在线固相萃取柱（MCX）在3 m L/min涡流下富集,5%氨水甲醇-水（9∶1）洗脱,采用CAPCELL MGⅡ液相色谱柱（150 mm×2.0 mm,3.0μm）分离,0.1%甲酸甲醇-0.1%甲酸（含5 mmol/L甲酸铵）为流动相,电喷雾正离子化监测模式下检测。在该实验条件下,16种β受体激动剂在0.01~50μg/L浓度范围内与峰面积呈良好的线性关系,相关系数（r2）不小于0.998 3,检出限（LOD）为0.01~0.025μg/L,定量下限（LOQ）为0.025~0.10μg/L;方法的回收率为62.4%~117.1%,相对标准偏差（RSD）为3.9%~16.3%。将方法用于213份猪尿液中β受体激动剂残留的检测,测定结果表明该方法灵敏、简单,可用于批量猪尿液中16种β受体激动剂的快速确证分析。
An automatic analysis method was dues including orciprenaline, clorprenaline, developed for the determination of 16 β-agonists resi- eimaterol, terbutaline, tulobuterol, cimbuterol, sal- butamol, zilpaterol, clenbuterol, ractopamine, fenoterol, mabuterol, bromochlorobuterol, mapen- terol, phenylethanolamine A and brombuterol in pig urine by liquid chromatography - tandem mass spectrometry（ LC - MS/MS）. The sample was digested overnight at 37 ℃, and purified by turboflow online cation solid-phase exaction （ online - MCX - SPE） at a flow rate of 3 mL/min. The elution was selected with 5% ammonium in methanol -water（9 ： 1 ）. The separation of 16 compounds was car- fled out on a CAPCELL MG II chromatographic column, using 0. 1% formic acid methanol -0. 1% formic acid solution containing 5 mmol/L ammonium formate as mobile phase, and determined in positive electro - spray ionization mode. Under the optimized conditions, the calibration curves of 16 agonists were linear in the concentration range of 0. 01 -50 μg/L with correlation coefficients（ r2） not less than 0. 998 3. The limits of detection（LOD） were in the range of 0. 01 - 0. 025 μg/L and the limits of quantitation （LOQ） were 0. 025 - 0. 10 μg/L. The recoveries of the method ranged from 62.4% to 117. 1% with relative standard deviations（RSDs） of 3.9% -16. 3%. The determination of 213 pig urines demonstrated that the method was simple and automatic, and was suitable for the quick confirmation of 16 β-agonists in large batch of pig urines.
出处
《分析测试学报》
CAS
CSCD
北大核心
2015年第7期802-806,812,共6页
Journal of Instrumental Analysis
基金
河南省重大科技攻关项目(121100110800)
河南省科技攻关项目(122102310456
122102210393)
关键词
阳离子涡流在线固相萃取
液相色谱-质谱/质谱
β受体激动剂残留
猪尿液
turboflow cation online solid phase extraction（ online -MCX -SPE）
liquid chromatog-raphy - tandem mass spectrometry（ LC - MS/MS）
β-agonist residues
pig urine
