液相色谱-串联质谱法测定焙炒咖啡中丙烯酰胺残留  

Determination of Acrylamide Residues in Roasted Coffee by Liquid Chromatography-tandem Mass Spectrometry

作　　者：毛静春 周琴 李宗师 蒲泓君 金红芳 李莲 王丽芳 王筱楠 程龙 MAO Jing-chun;ZHOU Qin;LI Zong-shi(Pu’er Institute of Inspection and Testing,Pu’er,Yunnan 665099)

机构地区：[1]普洱市检验检测院,云南普洱665099 [2]上海爱博才思分析仪器贸易有限公司,上海200335

出　　处：《安徽农业科学》2025年第4期174-177,共4页Journal of Anhui Agricultural Sciences

基　　金：云南省市场监督管理局科技计划项目(2022YSJK14)。

摘　　要：[目的]建立液相色谱-串联质谱法(LC-MS/MS)测定焙炒咖啡中丙烯酰胺的分析方法。[方法]以^(13)C_(3)-丙烯酰胺为内标物,样品经超纯水超声浸提,分别经正己烷萃取提取物脂肪、K_(4)Fe(CN)_(6)·3H_(2)O和Zn(CH_(3)COO)_(2)沉淀蛋白质、硅藻土和GCB净化等流程获取目标分析物,目标分析物最后经乙酸乙酯萃取浓缩,LC-MS/MS在ESI电离模式下测定丙烯酰胺含量。[结果]丙烯酰胺在10~500 ng/mL具有良好的线性关系(r=0.9999),在50、100、400μg/kg加标水平下回收率为71.2%~97.3%,RSD为1.9%~8.4%,方法检出限和定量限分别为13和40μg/kg。采用该方法对FAPAS质控样进行测定,检测结果均在质控值范围内。[结论]该方法具有良好的线性关系,准确度和精密度均满足定量分析的要求,适用于焙炒咖啡中丙烯酰胺残留的定量分析。[Objective] To establish an analytical method for the determination of acrylamide in roasted coffee by liquid chromatography-tandem mass spectrometry(LC-MS/MS).[Method]Taking ~(13)C_3-acrylamide as the internal standard,the coffee samples were extracted with ultra-pure water under ultrasonic,a cleanup by n-hexane extraction,K_4Fe(CN)_6·3H_(2O) and Zn(CH_3COO)_(2) precipitation,diatomite and GCB purification were employed to remove fat,protein and some interfering matrix compounds,respectively.The target analyte was finally extracted and concentrated with ethyl acetate,and the acrylamide content was determined by LC-MS/MS in ESI ionization mode.[Result]Acrylamide had a good linear relationship between 10-500 ng/mL(r=0.999 9),with recovery rates of 71.2%-97.3% and RSD of 1.9%-8.4% at spiked levels of 50,100 and 400 μg/kg.The detection limit and quantification limit of the method were 13 and 40 μg/kg,respectively.The method was used to determine the quality control samples of FAPAS,and the test results were all within the range of quality control values.[Conclusion]This method has a good linear relationship,and both accuracy and precision meet the requirements of quantitative analysis.It is suitable for the quantitative analysis of acrylamide residues in roasted coffee.

关 键 词：液相色谱-串联质谱法 焙炒咖啡 丙烯酰胺 残留 

分 类 号：TS207[轻工技术与工程—食品科学]