酱油生产过程中游离态羧甲基赖氨酸和5-羟甲基糠醛的同步检测

Simultaneous detection of free Nε-(carboxymethyl)lysine and 5-hydroxymethylfurfural in soy sauce production

为快速检测酱油生产过程中2种危害物羧甲基赖氨酸(CML)和5-羟甲基糠醛(5-HMF)的含量变化,采用高效液相色谱质谱联用(HPLC-MS/MS)技术建立了一种同步检测游离态CML和5-HMF的方法。通过质谱参数、色谱条件和前处理的优化,CML和5-HMF的回收率可达98%以上,样品中CML和5-HMF的检测限(LOD)分别为0.3ng/mL和6.0ng/mL,定量限(LOQ)分别为1.0ng/mL和20.0ng/mL。对酱油生产过程中各工艺工段的样品进行检测,发现发酵原料大曲中CML含量较高,而豆粕的蒸煮过程和老抽酱油的调配是使5-HMF含量增高的关键生产环节。

The high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) was used to investigate the changes in the contents of two hazardous components,Nε-(carboxymethyl)lysine (CML) and 5-hydroxymethylfurfural (5-HMF),during soy sauce production.Through mass spectrometry parameters,chromatographic conditions and pretreatment optimization,a method was established for simultaneous detection of free CML and 5-HMF.The results showed that the recovery of CML and 5-HMF was more than 98%,and the detection limits (LOD) of CML and 5-HMF in the samples were 0.3 ng/mL and 6 ng/mL respectively,the limits (LOQ) of which were 1 ng/mL and 20 ng/mL.In view of the detection results of CML and 5-HMF content in the process of soy sauce production,the content of CML in the fermentation raw material,distiller's yeast,is higher.And the stewing process of soybean pulp and the blending of soy sauce are the key links to increase the content of 5-HMF.