摘要
本文建立了酵母抽提物中9种黄色合成色素的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品用乙腈-甲醇(5∶5,V/V)提取,经聚苯乙烯/二乙烯苯(PEP)和C18粉净化,以Zorbax Eclipse Plus C18柱(100×3.0mm,1.8μm)分离,流动相为乙腈-10mmol/L NH4Ac,梯度洗脱。采用电喷雾负离子源(ESI-)、多重反应监测(MRM)模式检测,基质匹配外标法定量。结果表明,9种黄色合成色素在各自线性范围内相关系数(r2)均大于0.994;检出限(S/N〉3)为0.01-0.30mg/kg,定量限(S/N〉10)为0.02-3.0mg/kg,3个加标水平(1、2、10倍定量限)下,回收率为75.5%-115.1%,相对标准偏差(RSD)为4.7%-17.6%。该方法适用于酵母抽提物中9种黄色合成色素的同时测定。
A method was developed for the determination of nine yellow synthetic pigments in yeast extract by using QuEChERS-high performance liquid chromatography coupled with tandem mass spectrometry(HPLC-MS/MS).The samples were extracted by acetonitrile-methanol(5∶5,V/V),and then cleaned up by PEP and C18.The analytes were separated on a Zorbax Eclipse Plus C18column(100×3.0mm,1.8μm)by gradient elution with acetonitrile-10mmol/L ammonium acetate as the mobile phase.Nine synthetic pigments were determined by electrospray negative ion source(ESI-)with multiple reaction monitoring mode(MRM),and the quantitative analysis was carried out by matrix-matched external standard method.The calibration curves showed good linearity for nine synthetic pigments,and the correlation coefficients(r2)were greater than 0.994;the limits of quantification(LOQs,S/N10)were in the range of 0.02-3.0μg/kg.The average recoveries were in the range of 75.5%-115.1% for nine synthetic pigments with the relative standard deviations ranging from 4.7% to17.6% at the spiked levels of 1,2,10 LOQ.This method was suitable for the monitoring of nine yellow synthetic pigments in yeast extract.
出处
《分析科学学报》
CAS
CSCD
北大核心
2016年第2期234-238,共5页
Journal of Analytical Science
基金
国家质检总局科研项目(No.2014IK125)
作者简介
盂茹,女,工程师,主要从事酵母产品的质量安全研究.E—mail:rumeng5034@sina.com