气相色谱-质谱法测定咸味食品香精中3-氯-1,2-丙二醇  

Determination of 3-chloro-1,2-propandiol in savory flavoring by GC/MS

作　　者：唐熙[1] 刘华建 唐雯 邹哲祥 

机构地区：[1]福州大学石油化工学院,福建福州350108 [2]福建出入境检验检疫技术中心,福建福州350015

出　　处：《福建分析测试》2017年第1期1-6,共6页Fujian Analysis & Testing

基　　金：福建省科技计划重点项目(2011Y0001);国家质量监督检验检疫总局科技计划项目(2011IK028)

摘　　要：建立了一种可靠的测定咸味食品香精中3-氯-1,2-丙二醇(3-MCPD)的气相色谱-质谱(GC-MS)方法。考察了不同提取溶剂对香精中3-MCPD的提取效率;采用佛罗里硅土固相萃取柱净化样品,考察了不同比例的乙酸乙酯-正己烷淋洗液对3-MCPD回收率的影响,以及用七氟丁酸酐衍生时温度对产率的影响。本方法在1.0~10000μg/L的浓度范围内,3-MCPD有较好的线性关系,相关系数r>0.99。通过对不同类型的香精空白样品进行添加回收实验,精密度实验考察方法的可行性。3-MCPD的平均回收率介于89.4%~103%之间,相对标准偏差介于1.17%~4.33%。方法检出限为1.0μg/kg;定量限为5.0μg/kg。A method of determination of 3-chloro- 1,2-propandiol （3-MCPD） in savory flavoring by GC/MS was estab- lished.The effects of extraction （e.g.extraction solvent, extraction method） were carefully investigated. The method choose florisil solid extraction column to purify the extraction liquid, and the proportion of elution volume（ethyl acetate/hexane, V/ V） ＂affecting on recoveries of 3-MCPD were comparated. The eluent was derivated with heptafluorobutyric anhydride （HF- BA） , and the different derivate tempretures were examined. The linear range was from 1.0 μg/L to 10000 μg/L for3- MCPD, the correlation coefficients （r） of the calibration curves were above 0.99. The recoveries and the relative standard deviations of 3-MCPD in different kinds of food additives were investigated. The recoveries ranged from 89.4% - 103% and the relative standard deviations （RSDs） betweenl.17% - 4.33% （n=6）. The limits of detection（LODs） were in the range of 1.0 μg/kg, and the limits of quantitation （LOQs） were in the range of 5.0 μg/kg.

关 键 词：3-氯-1 2-丙二醇 咸味食品香精 气相色谱-质谱法 

分 类 号：TS264.21[轻工技术与工程—发酵工程]