顶空固相微萃取结合GC-MS测定酱油中的羟甲基糠醛衍生物  

Determination of Hydroxymethyl Furfural Derivatives in Soy Sauce by Headspace Solid-phase Microextraction Coupled with Gas Chromatography-mass Spectrometry

作　　者：万博恺 李丹丹 倪辉 杨远帆 黄高凌 WAN Bo-kai;LI Dan-dan;NI Hui;YANG Yuan-fan;HUANG Gao-ling(College of Food and Biological Engineering,Jimei University,Xiamen 361021,China;Key Laboratory of Food Microbiology and Enzyme Engineering Technology of Fuj ian Province,Xiamen 361021,China;Research Center of Food Biotechnology of Xiamen city,Xiamen 361021,China)

机构地区：[1]集美大学食品与生物工程学院,福建厦门361021 [2]福建省食品微生物与酶工程重点实验室,福建厦门361021 [3]厦门市食品生物工程技术研究中心,福建厦门361021

出　　处：《现代食品科技》2018年第9期208-214,共7页Modern Food Science and Technology

基　　金：国家自然科学基金项目(31271914)

摘　　要：为研究市售酱油中羟甲基糠醛衍生物的含量差异及评估其安全性,本文收集不同的酱油样品,应用顶空固相微萃取(SPME)结合气相色谱-串联质谱分析(GC-MS)检测其中的羟甲基糠醛衍生物。结果表明,从5种市售酱油中鉴定出3种羟甲基糠醛衍生物,分别为糠醛、2-乙基-1-己醇和5-甲基糠醛。它们在3.33~666.67μg/m L浓度范围内线性关系良好,检测限在3.33×10^(-1)μg/L以下,定量限在3.33μg/L及以下。加标回收率实验表明,对酱油直接进行SPME萃取分析回收率不符合国标要求,而将酱油用蒸馏水稀释5倍后进行SPME萃取分析回收率在82.23%~115.04%之间,日内准确度在93.31%~111.50%之间,日间准确度范围在93.02%~115.91%之间,日内精密度≤4.36%,日间精密度≤8.02%。五种酱油中糠醛含量在70.14~98.75μg/L之间,2-乙基-1-己醇含量在66.61~79.20μg/L之间,5-甲基糠醛含量在221.87~527.40μg/L之间。以上结果表明,虽然不同酱油中羟甲基糠醛衍生物含量有显著差异,但人们日常食用酱油的量,并不足以导致产生羟甲基糠醛衍生物的不良反应。In order to assay the content of hydroxymethylfurfural derivatives and evaluate the safety of soy sauces, five soy sauces that were collected in the local market were analyzed for the hydroxymethyl furfural derivatives by headspace solid-phase microextraction（SPME） combined with gas chromatography-tandem mass spectrometry（GC-MS）. As a result, three kinds of hydroxymethyl furfural derivatives, i.e., furfural, 5-methyl furfural and 2-ethyl-1-hexanol were identified. The linear regressive calibration curve was plotted within the concentration of 3.33-666.67 μg/m L with the LOD of 3.33×10^-1 μg/L and the LOQ of 3.33 g/L. The original soy sauce showed that the spiked recovery range was out of the national standard, and whereas the soy sauce after 5-fold dilution with distilled water had the recovery range between 82.23%-115.04%, with the inter-day recovery range between 93.31-111.50%. The inter-day recovery rate was ranged from 93.02% to 115.91%. The inter-day and intra-day precisions were 4.36% and 8.02%, respectively. The furfural content in the five soy sauces was between 70.14-98.75 μg/L, the 2-ethyl-1-hexanol content was between 66.61-79.20 μg/L, and the 5-methyl furfural content was between 221.87-527.40 μg/L. The above results indicated that the content of hydroxymethylfurfural derivatives were significantly different in different soy sauces. However, the daily consumption of soy sauce is safe because the intake of hydroxymethyl furfural derivatives is far below the bottom level to cause safety problems.

关 键 词：顶空固相微萃取 气相色谱-串联质谱法 酱油 糠醛 5-甲基糠醛 2-乙基-1-己醇 

分 类 号：TS264.21[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]