摘要
在测定酱油中苯甲酸过程中,目标峰附近会出现杂质峰,干扰积分进而影响定量。本文采用超高液相色谱法,对用乙醚提取酱油中苯甲酸和用固相萃取法过滤杂质两种提取方式进行对比。在0.01~1.0μg范围内,苯甲酸呈良好的线性关系,相关系数(r)为1;乙醚提取法苯甲酸的回收率为91.34~99.67%,该方法涉及试剂少、处理简单、检测快速准确、易用于实际样品的测定,同时加标回收率更高;固相萃取法苯甲酸的回收率为85.64~93.40%,该方法不需使用毒性大的试剂,分离效果好,基质干扰少,基线平稳更有利于积分。同时,采用超高液相法,苯甲酸出峰在2.3min左右,相较于高效液相色谱法提速近3倍。在实际应用上适合大批量检验任务。
During the determination of benzoic acid in soy sauce,impurity peaks appear near the target peak,which interfere with the integral and then affect the quantification.Ultra-high performance liquid chromatography(Ultra-high performance liquid chromatography)was used to compare the extraction methods of benzoic acid from soy sauce with ether and solid phase extraction(SPE)to filter impurities.In the range of 0.01-1.0 ug,the correlation coefficient(r)is1.The recovery of benzoic acid by ether extraction method is 91.34-99.67%.This method involves less reagents,simple treatment,rapid and accurate detection,and is easy to be used for the determination of actual samples.The recovery rate of benzoic acid by solid phase extraction is 85.64-93.40%.This method does not need to be used with high toxicity.The reagent has good separation effect,less matrix interference,and stable baseline is more conducive to integration.At the same time,the peak of benzoic acid was about 2.3 minutes by ultra-high performance liquid chromatography,which was nearly three times faster than that by high performance liquid chromatography.In practical application,it is suitable for mass inspection task.
作者
魏然
孙艳波
WEI Ran;SUN Yan-bo(Puyang Food and Drug Inspection and Testing Center,Puyang Henan 457000,China)
出处
《科技视界》
2019年第12期11-13,共3页
Science & Technology Vision
关键词
超高液相色谱法
酱油
乙醚
固相萃取
Ultra Performance Liquid Chromatography
Soy sauce
Ether
Solid phase
