摘要
本研究对气相色谱、质谱条件以及前处理方法进行优化,测定菜籽油中17种邻苯二甲酸酯(phthalic acid esters,PAEs)。结果表明,优化后最佳测定参数为初始温度80℃,进样口温度280℃,称样量1 g,氮吹温度60℃。优化后分离分析时间缩短,峰响应值加大且17种PAEs有较好的分离。在0.02~1.0μg·m L^(-1)的浓度范围内17种PAEs具有良好的线性关系,相关系数r≥0.997 8。检出限为0.002~0.02 mg·kg^(-1),定量限为0.005~0.06 mg·kg^(-1),远低于国家标准。相对标准偏差(RSD)为0.5%~9.6%,平均回收率在80.6%~118.3%,具有较高的精密度和准确度,优化后的方法高效、简单、快速,可为菜籽油中邻苯二甲酸酯的检测提供方法参考。
In this study,gas chromatography,mass spectrometry conditions and pretreatment methods were optimized to determine 17 phthalic acid esters(PAEs)in rapeseed oil.The results show that the optimal measurement parameters after optimization are the initial temperature of 80℃,the inlet temperature of 280℃,the weighing amount of 1 g,and the nitrogen blowing temperature of 60℃.After optimization,the separation and analysis time is shortened,the peak response value is increased,and the 17 PAEs are well separated.In the concentration range of 0.02~1.0μg·mL^(-1),the 17 PAEs have a good linear relationship,and the correlation coefficient is r≥0.9978.The detection limit is 0.002~0.02 mg·kg^(-1),and the quantification limit is 0.005~0.06 mg·kg^(-1),which is far lower than the national standard.The relative standard deviation(RSD)is 0.5%~9.6%,and the average recovery rate is between 80.6%~118.3%.It has high precision and accuracy.The optimized method is efficient,simple and fast,and can be rapeseed oil.Provide method reference for detection of phthalates.
作者
苟怡
王霓
熊双丽
吴秋婷
何建琼
GOU Yi;WANG Ni;XIONG Shuangli;Wu Qiuting;HE Jianqiong(Mianyang Product Quality Supervision and Inspection Institute,Mianyang 621000,China;College of Life Science and Engineering,Southwest University of Science and Technology,Mianyang 621010,China;Sichuan Tourism University,Chengdu 610000,China;Sichuan Yukang Agricultural Science and Technology Co.,Ltd.,Deyang 618500,China)
出处
《现代食品》
2021年第2期196-201,共6页
Modern Food
基金
菜籽油提质保香技术开发与应用研究(编号:19zd3120)。
