旋涡混合辅助超声提取-气质联用法分析食品添加剂中的咪唑.PDF

238 2013, Vol.34, No.24 食品科学 ※分析检测 旋涡混合辅助超声提取-气质联用法分析 食品添加剂中的咪唑 廖惠云，刘献军，庄亚东，张 映，熊晓敏，朱龙杰，李朝建，王珂清 (江苏中烟工业有限责任公司，江苏 南京 2100 19) 摘  要：建立旋涡混合辅助超声提取-气质联用法测定食品添加剂中咪唑的分析方法。采用旋涡混合器混合样品，使 样品基质均匀分散于萃取溶剂中，再使用超声从基质中提取目标物，探讨萃取溶剂种类及超声时间等因素对目标物萃 取效率的影响；之后甄选出合适的内标物，确定较佳的特征离子及其丰度比，分析进样量及分流比对目标物分离的影 响，得到了合适的色谱分析条件。在优化的实验条件下，目标物咪唑在0.1～4.0μg/mL范围内具有良好的线性关系，相 关系数(R2)为0.9997，平均回收率为89.82%～109.20%，相对标准偏差(RSD)为1.97%～2.28%，检出限为0.20mg/kg，定 量限为0.67mg/kg 。结果表明：该方法简便、快速、灵敏、准确，适合于食品添加剂中咪唑含量的测定。 关键词：旋涡混合；超声提取；气质联用；咪唑；食品添加剂 Determination of Imidazole in Food Additives by Using Vortex Mixing Coupled with Ultrasonic Extraction and GC-MS LIAO Hui-yun，LIU Xian-jun，ZHUANG Ya-dong，ZHANG Ying，XIONG Xiao-min，ZHU Long-jie，LI Chao-jian，WANG Ke-qing (China Tobacco Jiangsu Industry Co. Ltd., Nanj ing 2100 19, China) Abstract ：A gas chromatography-mass spectrometry method by using vortex mixing coupled with ultrasonic extraction was developed for the rapid determination of imidazole (IM) in food additives. In order to disperse the sample matrix into the extraction solvent, samples were homogenized by using a vortex mixer, and then extracted on an ultrasonic generator. The effect of solvent type and extraction time on the extraction efficiency of the analyte was discussed. Then, the appropriate internal standard was selected. The characteristic ions and their abundance were determined. Chromatography conditions such as inj ection volume and split ratio were optimized. Under the optimal conditions established in this study, the calibration range of IM was in the range of 0.1–4.0 μg/mL with a correlation coefficient of 0.9997, the average recoveries were in the range of 89.82%– 109.20% with relative standard deviat