河南出入境检验检疫局
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祝伟霞, 杨冀州, 郭慧领, 等. 阳离子涡流在线固相萃取/液相色谱-串联质谱快速分析猪尿液中16种β受体激动剂残留[J]. 分析测试学报, 2015,34(7):802-806.
Quick Determination of 16 β-Agonist Residues in Pig Urine by Turboflow Cation Online Solid Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry[J]. 2015,34(7):802-806.
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 mL/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,3.0 μm)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 ~50 μg/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 0.01~0.025 μg/L,定量下限(LOQ)为0.025 ~0.10 μg/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 developed for the determination of 16 β-agonists residues including orciprenaline,clorprenaline,cimaterol,terbutaline,tulobuterol,cimbuterol,salbutamol,zilpaterol,clenbuterol,ractopamine,fenoterol,mabuterol,bromochlorobuterol,mapenterol,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 carried out on a CAPCELL MGⅡ chromatographic column,using 0.1% formic acid methanol-01% 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.
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 chromatography-tandem mass spectrometry(LC-MS/MS)β-agonist residuespig urine
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