固相萃取-高效液相色谱串联质谱法同时检测辣椒粉中4种碱性染料  

Simultaneous determination of four alkaline dyes in foods by solid phase extraction - high performance liquid chromatography-tandem mass spectrometry

作　　者：黄优生[1] 罗香[1] 熊华亮[1] 肖庚鹏[1] 

机构地区：[1]江西省分析测试研究所,南昌330029

出　　处：《分析试验室》2013年第10期72-76,共5页Chinese Journal of Analysis Laboratory

基　　金：江西省科技支撑计划项目(20132BBG70102)资助

摘　　要：建立了固相萃取-液相色谱串联质谱法同时检测辣椒粉中罗丹明B、碱性橙2、碱性橙21、碱性橙22的分析方法。样品经甲醇提取,MCX和WCX弱阳离子交换固相萃取柱净化,采用液相色谱分离、多反应监测模式进行检测,基质曲线外标法定量。结果表明,罗丹明B、碱性橙21、碱性橙22的定量限为0.25μg/kg,碱性橙2的定量限为0.50μg/kg,4种染料的线性范围为0.2～50μg/L,线性相关系数均大于0.9990。4种染料在5,10,50μg/kg 3个添加水平范围内的回收率为73.2%～102.3%,相对标准偏差为2.8%～9.1%。方法适合于辣椒粉中4种碱性染料的定量分析。An analytical method was developed for the simultaneous determination of 4 alkaline dyes（Rhodamine B、Basic Orange 2、Basic Orange 21 and Basic Orange 22） in chili powders based on solid phase extraction followed by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS / MS）.The samples were extracted with methanol,purified by MCX and WCX solid phase extraction column.The target analytes were separated on a RP-HPLC column and analyzed in multiple reaction monitoring（MRM） mode.Sample matrix-matched calibration was used to determine the residue contents by external standard.Limits of quantitation（LOQ） of rhodamine B、basic orange 21 and Basic Orange 22 were 0.25μg/kg and that of basic orange 2 was 0.50μg / kg,the linear ranges were 0.2 ～ 50μg / L with correlation coefficients larger than 0.9990.The recoveries of 4 dyes ranged from chili powders spiked with the concentration levels at 5,10,50μg / kg ranged from 73.2% to 102.3% with relative standard deviations（RSD） of 2.8% ～ 9.1%.This method was simple,effective and sensitive,and was suitable for the determination and confirmation of four alkaline dyes added in chili powders.

关 键 词：高效液相色谱-串联质谱法 固相萃取 碱性染料 辣椒粉 

分 类 号：O657.63[理学—分析化学]