分散固相萃取-HPLC及UPLC-MS/MS法测定豆干和调味品中的二甲基黄和二乙基黄

doi:10.7506/spkx1002-6630-201608039

食品科学

分散固相萃取-HPLC及UPLC-MS/MS法测定豆干和调味品中的二甲基黄和二乙基黄

林子豪1,2，周庆琼1，曾羲1，郑春浩1，黄思铭2，欧阳钢锋2，戚平1,*

1.广州市食品检验所，广东广州 510410；2.中山大学化学与化学工程学院，广东广州 510275

出版日期:2016-04-25 发布日期:2016-04-13

Determination of Dimethyl Yellow and Diethyl Yellow in Dried Beancurd and Condiment Using Dispersive Solid-Phase Extraction and HPLC with Diode Array Detector and UPLC-MS/MS

LIN Zihao1,2, ZHOU Qingqiong1, ZENG Xi1, ZHENG Chunhao1, HUANG Siming2, OUYANG Gangfeng2, QI Ping1,*

1. Guangzhou Institute for Food Control, Guangzhou 510410, China；
2. School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China

Online:2016-04-25 Published:2016-04-13

摘要/Abstract

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。

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

Abstract:

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 C18 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.

Key words: dimethyl yellow, diethyl yellow, high performance liquid chromatography (HPLC), ultra high performance liquid chromatography-mass spectrometry (UPLC-MS/MS), dried beancurd, condiment

中图分类号:

O657

林子豪，周庆琼，曾羲，郑春浩，黄思铭，欧阳钢锋，戚平. 分散固相萃取-HPLC及UPLC-MS/MS法测定豆干和调味品中的二甲基黄和二乙基黄[J]. 食品科学, doi: 10.7506/spkx1002-6630-201608039.

LIN Zihao, ZHOU Qingqiong, ZENG Xi, ZHENG Chunhao, HUANG Siming, OUYANG Gangfeng, QI Ping. Determination of Dimethyl Yellow and Diethyl Yellow in Dried Beancurd and Condiment Using Dispersive Solid-Phase Extraction and HPLC with Diode Array Detector and UPLC-MS/MS[J]. FOOD SCIENCE, doi: 10.7506/spkx1002-6630-201608039.

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分散固相萃取-HPLC及UPLC-MS/MS法测定豆干和调味品中的二甲基黄和二乙基黄

Determination of Dimethyl Yellow and Diethyl Yellow in Dried Beancurd and Condiment Using Dispersive Solid-Phase Extraction and HPLC with Diode Array Detector and UPLC-MS/MS

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