气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺

doi:10.3864/j.issn.0578-1752.2012.16.017

中国农业科学 ›› 2012, Vol. 45 ›› Issue (16): 3373-3381.doi: 10.3864/j.issn.0578-1752.2012.16.017

气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺

程劼, 苏晓鸥, 张维, 王瑞国, 王培龙, 李阳

中国农业科学院农业质量标准与检测技术研究所，北京100081

收稿日期:2011-11-28 出版日期:2012-08-15 发布日期:2012-05-31
通讯作者: 通信作者苏晓鸥，Tel：010-82106307；E-mail：suxiaoou@caas.net.cn
作者简介:程劼，Tel：010-82106576；E-mail：chengjie17@163.com
基金资助:
农业部“餐厨废弃物饲料化利用安全评价”专项（2130112）

Determination of Acrylamide in Kitchen Waste Using Gas Chromatography-Tandem Mass Spectrometry

CHENG Jie, SU Xiao-鸥, ZHANG Wei, WANG Rui-Guo, WANG Pei-Long, LI Yang

中国农业科学院农业质量标准与检测技术研究所，北京100081

Received:2011-11-28 Online:2012-08-15 Published:2012-05-31

摘要/Abstract

摘要： 【目的】建立气相色谱-串联四极杆质谱（GC/MS/MS）检测餐厨废弃物中的丙烯酰胺。【方法】样品经去离子温水提取结合C18 SPE小柱净化或者经甲酸溶液提取/Carrez试剂预处理，MCX柱净化的两种前处理方法进行前处理，然后经过衍生反应，利用气相色谱串联三重四极杆质谱检测，在SRM检测模式下，以离子对m/z 152＞135和m/z 152＞107为定性离子对，m/z 152＞135为定量离子，碰撞气体能量15 V，外标法定量。【结果】该方法在3.0—30 ng•L-1浓度中呈现良好的线性关系，相关系数R2=0.9984，丙烯酰胺的检出限值为1.0 ng•g-1（S/N=3），回收率为95.3%—108.1%，3个水平添加下的相对标准偏差（RSD）均小于4.3%。【结论】所建立的方法稳定、灵敏度高，可用于餐厨废弃物中丙烯酰胺的测定。

关键词: 气相色谱-串联四极杆质谱, 餐厨废弃物, 丙烯酰胺

Abstract: 【Objective】The objective of this study is to develop an analysis methods of the acrylamide in kitchen waste using gas chromatography-tandem mass spectrometry.【Method】The use of warm deionized water extraction and C18 SPE clean-up or the formic acid extraction and Carrez reagent/MCX clean-up as the sorbented appeared to be a very effective sample preparation method. After derivative reaction, gas chromatography-tandem mass spectrometry was used to detect the sample in the mode of SRM, and the external standard method was used for quantitative analysis. The qualitative ion is m/z 152＞135 and 152＞107 and the quantitative ion is m/z 152＞135. The pressure of gas collision is 15V.【Result】The developed method presented a good linearity from 3 ng•L-1 to 30 ng•L-1 with the correlation coefficient of 0.9984. The RSD of the method was 4.3% and of the quantitative limit was 1.0 ng•g-1. The rate of recovery was 95.3%-108.1%.【Conclusion】The developed method is a very effective method for detecting the acrylamide in kitchen waste.

Key words: gas chromatography-tandem mass, kitchen waste, acrylamide

程劼, 苏晓鸥, 张维, 王瑞国, 王培龙, 李阳. 气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺[J]. 中国农业科学, 2012, 45(16): 3373-3381.

CHENG Jie, SU Xiao-鸥, ZHANG Wei, WANG Rui-Guo, WANG Pei-Long, LI Yang. Determination of Acrylamide in Kitchen Waste Using Gas Chromatography-Tandem Mass Spectrometry[J]. Scientia Agricultura Sinica, 2012, 45(16): 3373-3381.

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气相色谱-串联四极杆质谱测定餐厨废弃物中的丙烯酰胺

Determination of Acrylamide in Kitchen Waste Using Gas Chromatography-Tandem Mass Spectrometry

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