超快速液相色谱-离子阱飞行时间质谱法测定肉制品中10种碱性染料  

Determination of ten basic dyes in meat products by ultra fast liquid chromatography-ion trap time of flight mass spectrometry

作　　者：张东雷 汪丽娜[2] 陈小珍 王瑾 曹慧 黄丽英 

机构地区：[1]浙江省质量检测科学研究院,浙江杭州310013 [2]浙江工业大学化学工程与材料学院,浙江杭州310014

出　　处：《色谱》2012年第8期770-776,共7页Chinese Journal of Chromatography

基　　金：浙江省质量技术监督系统科研计划项目(20100104);浙江省公益性技术应用研究(分析测试)项目(2011C37048)

摘　　要：建立了肉制品中10种碱性染料的超快速液相色谱-离子阱飞行时间质谱(LC-IT-TOF-MS)检测方法。使用Waters AcquityTM UPLC BEH C18(100mm×2.1mm,1.7μm)作为分析柱,以5mmol/L乙酸铵水溶液-含0.1%(体积分数)甲酸的乙腈溶液为流动相进行梯度洗脱,流速0.2mL/min。采用电喷雾离子化源,在正离子模式下进行检测。样品用乙腈提取,经弱阳离子交换(Oasis WCX)固相萃取柱净化,超快速液相色谱分离,外标法定量。结果表明,10种碱性染料在1.0～100.0μg/L范围内线性关系良好,r2均大于0.991 5,相对标准偏差(n=7)均小于8.54%。在2,10,25μg/kg 3个添加水平下平均回收率为65.39%～119.18%。该方法简单、灵敏度高、分析时间短,适用于肉制品中多种碱性染料的同时测定。A method was developed for the simultaneous determination of 10 basic dyes in meat products using ultra fast liquid chromatography-ion trap time of flight mass spectrometry（LC-IT-TOF-MS）.The target analytes were separated at a flow rate of 0.2 mL/min on a Waters AcquityTM UPLC BEH C18（100 mm×2.1 mm,1.7 μm） column with a gradient elution.The mobile phase was 5 mmol/L ammonium acetate-acetonitrile（containing 0.1%（v/v） formic acid）.The identification and quantification were achieved in positive ion mode with electro spray ionization source.The samples were extracted with a simple procedure using acetonitrile and cleaned up by weak cation exchange（Oasis WCX）solid phase extraction column.Ten basic dyes were determined by LC-IT-TOF-MS,and quantified by external standard method.The developed method showed a good linearity over the wide range of 1.0-100.0 μg/L,and the relative standard deviations（n=7） were less than 8.54%.The average recoveries of the ten basic dyes at three levels（2,10 and 25 μg/kg） were ranged from 65.39% to 119.18%.Therefore,this method,owing to its simplicity,rapidity and high sensitivity,has a good applicability to the simultaneous determination of dye residues in meat products.

关 键 词：超快速液相色谱-离子阱飞行时间质谱 碱性染料 肉制品 

分 类 号：O658[理学—分析化学]