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采用固相萃取和气相色谱-三重四极杆质谱联用技术测定中式烹饪食品中痕量食品源有害化合物

Determination of trace food-derived hazardous compounds in Chinese cooked foods using solid-phase extraction and gas chromatography coupled to triple quadrupole mass spectrometry.

作者信息

Zhang Feng, Chu Xiaogang, Sun Li, Zhao Yansheng, Ling Yun, Wang Xiujuan, Yong Wei, Yang Minli, Li Xiuqin

机构信息

Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Jia 3 Gaobeidianbei Road, Beijing 100123, China.

出版信息

J Chromatogr A. 2008 Oct 31;1209(1-2):220-9. doi: 10.1016/j.chroma.2008.09.012. Epub 2008 Sep 7.

Abstract

Gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) with a triple quadrupole analyzer (QqQ) was applied for the first time to the determination of trace food-derived hazardous compounds in food samples. Thirteen heterocyclic amines were confirmed and quantified by the developed sensitive method. The method includes a solid-phase extraction procedure with a polystyrene copolymer cartridge (LiChrolut EN), followed by a derivatization reaction with N,N-dimethylformamide di-tert-butylacetal. Analyses were performed by gas chromatography with triple quadrupole mass spectrometry in the electron impact mode. The MS/MS fragmentation pathway of derived heterocyclic amines was studied and the differences of fragmentation characteristics were used successively to distinguish the isomers in absence of chemical standards. The excellent selectivity and sensitivity achieved in multiple reaction monitoring mode allowed us satisfactory quantitation and confirmation. The limits of quantitation of the method for these compounds ranged from 0.12 to 0.48ng/g of sample. The method developed was applied to the analysis of Chinese cooked foods, and the results demonstrated the potentiality of the GC-MS/MS method for the analysis of trace food-derived hazardous compounds in complex food matrices such as meat samples.

摘要

首次将配备三重四极杆分析仪(QqQ)的气相色谱-串联质谱联用仪(GC-MS/MS)用于测定食品样品中痕量的食品源有害化合物。通过所开发的灵敏方法对13种杂环胺进行了确证和定量。该方法包括使用聚苯乙烯共聚物柱(LiChrolut EN)进行固相萃取,随后与N,N-二甲基甲酰胺二叔丁基缩醛进行衍生化反应。采用气相色谱-三重四极杆质谱联用仪在电子轰击模式下进行分析。研究了衍生化杂环胺的MS/MS裂解途径,并利用裂解特征的差异依次区分了在没有化学标准品的情况下的异构体。在多反应监测模式下实现的出色选择性和灵敏度使我们能够进行令人满意的定量和确证。这些化合物的该方法定量限为0.12至0.48 ng/g样品。所开发的方法应用于中式烹饪食品的分析,结果证明了GC-MS/MS方法在分析肉类样品等复杂食品基质中痕量食品源有害化合物方面的潜力。

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