色谱 ›› 2015, Vol. 33 ›› Issue (6): 657-661.DOI: 10.3724/SP.J.1123.2015.01046

• 技术与应用 • 上一篇    下一篇

改进的QuEChERS方法结合液相色谱-串联质谱法测定腐竹和豆干中的二甲基黄和二乙基黄

范素芳, 李强, 马俊美, 李挥, 张岩   

  1. 河北省食品检验研究院, 河北省食品安全重点实验室, 河北 石家庄 050091
  • 收稿日期:2015-01-30 发布日期:2015-05-26
  • 通讯作者: 李强, 张岩

Determination of dimethyl yellow and diethyl yellow in yuba and dried beancurd by modified QuEChERS method and liquid chromatography-tandem mass spectrometry

FAN Sufang, LI Qiang, MA Junmei, LI Hui, ZHANG Yan   

  1. Hebei Food Inspection and Research Institute, Key Laboratory of Food Safety of Heibei Province, Shijiazhuang 050091, China
  • Received:2015-01-30 Published:2015-05-26

摘要:

建立了基于改进的QuEChERS方法结合液相色谱-串联质谱测定腐竹和豆干中二甲基黄和二乙基黄的方法。在2.0 g腐竹和豆干样品中加入5 mL水浸泡,然后加入10 mL乙腈提取,加入1.0 g NaCl、2.0 g无水硫酸镁进行液液分离;取1 mL提取液经50 mg N-丙基二乙胺分散固相萃取净化,经液相色谱分离、质谱测定,外标法定量。二甲基黄在添加水平为0.3、1和10 μg/kg时,方法的回收率为73.5%~84.5%;二乙基黄在添加水平为0.1、1和10 μg/kg时,方法的回收率为70.5%~81.2%;方法的相对标准偏差小于11%。二甲基黄的检出限和定量限分别为0.1 μg/kg和0.3 μg/kg,二乙基黄的检出限和定量限分别为0.05 μg/kg和0.1 μg/kg。该方法可以用于腐竹、豆干中二甲基黄和二乙基黄的快速筛查和定量分析。

关键词: QuEChERS, 豆干, 二甲基黄, 二乙基黄, 腐竹, 液相色谱-串联质谱

Abstract:

A modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method followed by liquid chromatography-tandem mass spectrometric analysis was developed for the determination of dimethyl yellow and diethyl yellow in yuba and dried beancurd. Yuba and dried beancurd samples were soaked by deionized water, then acetonitrile was added to extract the analytes. Sodium chloride and anhydrous magnesium sulfate were added for liquid-liquid separation. The extracts were cleaned-up by dispersive solid-phase using N-propyl diethylamine. The analytes were separated by liquid chromatography and determined by mass spectrometry. External standard method was used for quantification. The recoveries of dimethyl yellow were in the range of 73.5%-84.5% at spiked levels of 0.3, 1 and 10 μg/kg and the recoveries of diethyl yellow were in range of 70.5%-81.2% at spiked levels of 0.1, 1 and 10 μg/kg; relative standard deviations of the method were lower than 11%. The limit of detection and the limit of quantification of dimethyl yellow were 0.1 μg/kg and 0.3 μg/kg, respectively; the limit of detection and the limit of quantification of diethyl yellow were 0.05 μg/kg and 0.1 μg/kg, respectively. This method can be used in rapid screening and quantitative analysis of dimethyl yellow and diethyl yellow in yuba and dried beancurd.

Key words: diethyl yellow, dimethyl yellow, dried beancurd, liquid chromatography-tandem mass spectrometry (LC-MS/MS), QuEChERS, yuba

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