UPLC-Q-TOF/MS在烘焙食品中羧甲基赖氨酸和羧乙基赖氨酸检测中的应用

建立了烘焙食品中羧甲基赖氨酸(CML)和羧乙基赖氨酸(CEL)的UPLC-Q-TOF/MS检测方法。烘焙食品经脱脂、还原、沉淀蛋白、酸水解释放出CML和CEL,使用FMOC-Cl柱前衍生和HLB小柱固相萃取净化后,采用UPLC-Q-TOF/MS检测。CML和CEL在1~700 ng/m L浓度范围内均呈良好的线性关系,线性回归系数r0.999。CML和CEL的检出限均为0.1 mg/kg;回收率为94.4%~108.3%;相对标准偏差(RSD,n=6)为0.4%~6.2%。该方法定性、定量准确,灵敏度高,能很好地应用于烘焙食品中CML和CEL的检测。

Application of Ultra Performance Liquid Chromatography-Quadrupole Time-of-flight Mass Spectrometry in Determination of CML and CEL in Baking Foods

A method was developed for the determination of Nε-(carboxymethyl) lysine (CML) and Nε-(carboxyethyl) lysine(CEL) in baking food using ultra performance liquid chromatography-quadrupole Time-of-flight mass spectrometry(UPLC-Q-TOF/MS).CML and CEL were released from the baking foods through the process of sample degreasing,reduction reaction,precipitation and acid hydrolysis of acquired protein,treated by pre-column derivation with FMOC-Cl,and purified with HLB solid-phase extraction(SPE) column.Then the contents of CML and CEL in pretreated samples were determined by UPLC-Q-TOF/MS.All the target compounds exhibited good linearity (r ＞0.999) over the concentration range of 1-700 ng/mL.The detection limits of CML and CEL were all 0.1 mg/kg and the mean recoveries were in the range of 94.4％-108.3％ with relative standard deviations(RSD,n =6) of 0.4％-6.2％.The method was accurate and sensitive,and was suitable for the detection of CML and CEL contents in baking foods.