固相萃取/液相色谱-串联质谱法测定食品中二甲基黄  

Determination of dimethyl yellow in foods by liquid chromatography-tandem mass spectrometry coupled with solid phase extraction

作　　者：李优[1] 徐敦明[2] 伊雄海[1] 盛永刚[1] 时逸吟 赵善贞[1] 邓晓军[1] 

机构地区：[1]上海出入境检验检疫局,上海200135 [2]厦门出入境检验检疫局,福建厦门361026

出　　处：《色谱》2017年第4期398-404,共7页Chinese Journal of Chromatography

基　　金：国家重大科学仪器设备开发专项(2013YQ15055705);上海市技术性贸易措施应对专项(14TBT006,15TBT004,15TBT005);上海市科委技术标准专项(15DZ0503201);长三角科技合作项目(15395810100)~~

摘　　要：建立了液相色谱-串联质谱(LC-MS/MS)测定食品中二甲基黄(DMY)的分析方法。样品经乙酸乙酯提取,二甲基黄专用固相萃取小柱(ProElut DMY SPE)净化,XDB-C18色谱柱(50 mm×4.6 mm,1.8μm)分离,并以5mmol/L乙酸铵水溶液(含0.1%(v/v)甲酸)-乙腈(含0.1%(v/v)甲酸)为流动相,梯度洗脱,电喷雾正离子模式(ESI^+)电离,多反应监测模式(MRM)检测,内标法定量。结果表明,DMY在0~50μg/L范围内线性关系良好,相关系数(r^2)均大于0.999。方法的检出限(LOD,S/N>3)和定量限(LOQ,S/N>10)分别为2μg/kg和10μg/kg。不同食品基质中,DMY在10、20和100μg/kg的添加水平下的平均加标回收率为93.3%~98.9%,相对标准偏差为1.6%~3.9%(n=6)。该方法有效补偿了液相色谱-串联质谱检测过程中的离子化抑制效应,灵敏度和准确度高,适用于腐乳、辣椒酱、禽蛋、豆干、糖果和火腿中DMY的测定。A liquid chromatography-tandem mass spectrometry （LC-MS/MS） was established for the determination of dimethyl yellow （DMY） in foods. The samples spiked with D5-dimethyl yellow （D5-DMY） as the internal standard were extracted with ethyl acetate,cleaned up by a ProElut DMY SPE column. The separation was performed on an XDB-C18 column （50 mm ×4. 6 mm,1. 8μm） with the mobile phases of 5 mmo/ L ammonium acetate aqueous solution contai-ning 0. 1% （v/v） formic acid and acetonitrile containing 0. 1% （v/v） formic acid. The identifica-tion and quantitation of DMY was performed by MS/MS in positive electrospray ionization （ESI＋） and multiple reaction monitoring （MRM） mode. The quantitative analysis was carried out by internal standard method. A good linear relationship, with the correlation coefficient （r2） greater than 0. 999,was found in the mass concentration range of 0-50 μg/L. The limit of detection （LOD, S/N〉3） and the limit of quantitation （LOQ,S/N 〉10） were 2 μg/kg and 10 μg/kg, respectively. The recoveries of DMY in foods spiked with 10, 20 and 100 pg^kg varied from 93. 3% method can effectively correct the ionization suppression, and it is sensitive, accurate and suit-able for the monitoring of DMY in sufu, chili sauce, egg, dried bean curd, candy and ham.

关 键 词：液相色谱-串联质谱 固相萃取 内标法 基质效应 二甲基黄 食品 

分 类 号：O658[理学—分析化学]