生物炭萃取-高效液相色谱法测定对羟基苯甲酸酯类  

Determination of p-hydroxybenzoic acid esters extraction by biochar-high pressure liquid chromatography

作　　者：于娇娇[1] 李红霞 苏伟[3] 甘黎明[1] 李薇[1] YU Jiao-jiao;LI Hong-xia;SU Wei;GAN Li-ming;LI Wei(Lanzhou Petrochemical College of Vocational Technical,Lanzhou 730060;Quality Inspection Department of Lanzhou Petrochemical Company,Lanzhou 730060;School of Chemical Engineering and Technology,Tianjin University,Tianjin 300350)

机构地区：[1]兰州石化职业技术学院,兰州730060 [2]兰州石化公司质检部,兰州730060 [3]天津大学化工学院,天津300350

出　　处：《中国食品添加剂》2020年第5期82-86,共5页China Food Additives

基　　金：国家自然科学基金(21406004)。

摘　　要：目的:建立4种对羟基苯甲酸酯类(甲酯、乙酯、丙酯、丁酯)同时测定的生物炭萃取-高效液相色谱分析方法。方法:样品中的对羟基苯甲酸酯类经生物炭吸附-甲醇脱附,0.45μm有机微孔滤膜过滤后,用高效液相色谱法进行检测。结果:采用外标法测定,4种对羟基苯甲酸酯在0~200μg/mL范围内线性相关系数(r)≥0.997,检出限为0.9μg/mL^2.1μg/mL,加标回收率为87.1%~98.2%,相对标准偏差为2.3%~7.1%。采用本方法对3个厂家的小苏打水进行检测,均检出对羟基苯甲酸甲酯,其含量分别为16.82μg/mL、14.09μg/mL、24.18μg/mL,符合国家标准。结论:本方法适用于饮料中4种对羟基苯甲酸酯类的同时快速测定。Objective:To establish a fast and accurate method for determining of methyl p-hydroxybenzoic acid ester,ethyl p-hydroxybenzoic acid ester,propyl p-hydroxybenzoic acid ester and butyl p-hydroxybenzoic acid ester by combination of biochar extraction and high pressure liquid chromatography(HPLC)detection.Methods:The p-hydroxybenzoic acid esters were adsorbed by biochar,and desorbed by methanol,filtrated through 0.45μm filter membrane,and analyzed by HPLC.Results:The quantification was based on external standard curves.The method correlation coefficient is more than 0.997 for four p-hydroxybenzoic acid esters in the range of 0~200μg/m L.The limits of detection were within 0.9μg/mL^2.1μg/mL.The recovery rates were from 87.1%to 98.2%and the relative standard deviations were in the range of 2.3%~7.1%.Methyl p-hydroxybenzoate was detected in soda water from three manufacturers,and the content was 16.82μg/mL,14.09μg/mL and 24.18μg/mL respectively,which met the national standard.Conclusion:The method is suitable for simultaneous and rapid determination of four kinds of p-hydroxybenzoic acid esters in beverage.

关 键 词：生物炭吸附 高效液相色谱 对羟基苯甲酸酯类 

分 类 号：TS202.3[轻工技术与工程—食品科学] O657.72[轻工技术与工程—食品科学与工程]