气相色谱法测定酱油和食醋中对羟基苯甲酸酯的方法优化  

Optimization of Gas Chromatography Method for Determination of Paraben in Soy Sauce and Vinegar

作　　者：张悦 边文文 徐瑶 ZHANG Yue;BIAN Wenwen;XU Yao(Shaanxi Institute of Supervision&Testing on Product Quality,Xi'an,Shaanxi 710048,China)

机构地区：[1]陕西省产品质量监督检验研究院,陕西西安710048

出　　处：《农产品加工》2025年第6期60-63,69,共5页Farm Products Processing

摘　　要：通过选择试样提取溶剂、改变试样提取过程等方法,对气相色谱法测定酱油和食醋中对羟基苯甲酸酯类防腐剂的检测方法进行优化。采用优化后的方法对市售酱油和食醋中对羟基苯甲酸酯类防腐剂的含量进行测定。优化后的最佳条件:样品经充分混匀后加入水10 mL进行稀释,加入1∶1盐酸溶液1 mL,选用乙酸乙酯溶液5 mL提取后采用HP-5型毛细管色谱柱进行分离,最后经氢火焰离子化检测器FID检测。结果表明,在质量浓度4.0~300.0μg/mL内,4种对羟基苯甲酸酯类防腐剂的线性关系较好,相关系数均大于0.999;在0.6,2.0,6.0 mg/kg 3个不同质量浓度下,酱油基质中对羟基苯甲酸酯类防腐剂的回收率为95.1%~104.6%,食醋基质中对羟基苯甲酸酯类防腐剂的回收率为95.3%~104.6%,相对标准偏差(RSD)为1.80%~4.13%(n=6)。该方法易于操作且精密度高,可为食品中对羟基苯甲酸酯类防腐剂的风险监测提供准确的技术参考和理论依据。In this study,the gas chromatography method for the determination of preservatives in soy sauce and vinegar was optimized by selecting the extraction solvent and changing the extraction process of the paraben.The contents of paraben in commercial soy sauce and vinegar were determined by an optimized method.The optimum conditions were as follows:the samples were mixed well,diluted with 10 mL water,acidified with 1 mL,1∶1 hydrochloric acid,extracted with 5 mL ethyl acetate and separated by HP-5 capillary column,finally,it was detected by FID detector.The results showed that in the range of 4.0~300.0μg/mL,the linear relationships of the four paraben were better,and the correlation coefficients were higher than 0.999.At the addition levels of 0.6,2.0,6.0 mg/kg,the recoveries of paraben in soy sauce and vinegar were 95.1%~104.6%and 95.3%~104.6%,and the relative standard deviation(RSD)was 1.80%~4.13%(n=6).The method was easy to operate and has high precision,which provided accurate technical reference and theoretical basis for risk monitoring of paraben in food.

关 键 词：对羟基苯甲酸酯 气相色谱法 酱油 食醋 

分 类 号：O657[理学—分析化学]