摘要
建立豆干和调味品中二甲基黄、二乙基黄的高效液相色谱初步筛查方法和超高效液相色谱-串联质谱确证方法。样品用酸化乙腈提取,经旋转蒸发浓缩和分散固相萃取净化后,采用高效液相色谱仪进行筛查,遇到阳性样品时,结合超高效液相色谱-串联质谱法进行确证分析,并对方法的有效性进行验证。结果表明,在高、中、低3个水平进行加标回收实验,高效液相色谱法和超高效液相色谱-串联质谱法回收率分别在92.2%~102.6%和84.7%~110.7%之间,相对标准偏差分别为0.14%~6.71%和0.16%~6.43%。高效液相色谱法成本较低、操作简单,适用于样品的筛查工作;超高效液相色谱-串联质谱法灵敏度高、定性准确性强,适用于阳性样品的确证。
In this study,a fast and sensitive method for the simultaneous determination of dimethyl yellow and diethyl yellow in dried beancurd and condiment was developed and validated using HPLC coupled with diode array detector（DAD） and ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.The two dyes were extracted with hydrochloric acid-acetonitrile.The extracts were further purified with dispersive solid-phase extraction（dSPE） procedure using C_（18） to reduce matrix interference.The validation of the UPLC-DAD method was performed using HPLC-MS/MS.Good recoveries in the range of 84.7%-110.7%were obtained,with relative standard deviations less than 7%.The HPLC method was economical,simple and suitable for screening of samples,and the UPLC-MS/MS method was sensitive and accurate and suitable for validation of positive samples.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2016年第8期217-221,共5页
Food Science
基金
广州市科技计划项目(2014J4100196)
关键词
二甲基黄
二乙基黄
高效液相色谱法
超高效液相色谱-串联质谱法
豆干
调味品
dimethyl yellow
diethyl yellow
high performance liquid chromatography（HPLC）
ultra high performance liquid chromatography-mass spectrometry（UPLC-MS/MS）
dried beancurd
condiment
