摘要
建立食醋中对羟基苯甲酸甲、乙、丙、丁酯含量的高压梯度液相色谱分析方法.样品去蛋白后,用水提取,用高压液相色谱仪进行检测.对羟基苯甲酸甲、乙、丙酯质量浓度在0.25~100 mg/L范围内,相关系数大于0.999,对羟基苯甲酸丁酯含量在1.0~400 mg/L范围内,相关系数大于0.999.对羟基苯甲酸甲、乙、丙、丁酯检出限分别为1,1,0.8和2 mg/kg;在1,4,10和25 mg/kg这4个加标水平下,样品中对羟基苯甲酸甲、乙、丙、丁酯的加标回收率分别为95.59%~104.52%,93.21%~108.05%,97.75%~107.98%和97.48%~103.67%,相对标准偏差均小于5%(n=6).该方法适用于食醋中对羟基苯甲酸甲、乙、丙、丁酯含量的快速测定.
Abstract
A high-pressure gradient liquid chromatography method was established for the analysis of para hydroxybenzoatemethyl,ethyl,propyl,and butyl esters in vinegar.After removing the protein from the sample,it was extracted with water and detected using a high-pressure liquid chromatograph.The content of methyl,ethyl,and propyl hydroxybenzoate ranges from 0.25 mg/L to 100 mg/L,with a correlation coefficient greater than 0.999.The content of butyl hydroxybenzoate ranges from 1.0 mg/L to 400 mg/L,with a correlation coefficient greater than 0.999.The detection limits for methyl,ethyl,propyl,and butyl hydroxybenzoate were 1,1,0.8 and 3 mg/kg,respectively.At four spiking levels of 1,4,10 and 25 mg/kg,the spiked recoveries of methyl,ethyl,propyl,and butyl hydroxybenzoate in the samples were 95.59%-104.52%,93.21%-108.05%,97.75%-107.98%,and 97.48%-103.67%,respectively.The relative standard deviations were all less than 5%(n=6).This method was suitable for the rapid determination of para hydroxybenzoic methyl,ethyl,propyl,and butyl esters in vinegar.
基金项目
2023年陕西省市场监督管理局科技计划项目()
宝鸡擀面皮产业质量提升与加工关键技术研究(2023KY28)