超高效液相色谱法测定水产品保鲜剂中4-己基间苯二酚的含量  

Determination of 4-Hexylresorcinol in Aquatic Preservative by Ultra Performance Liquid Chromatography

作　　者：高学慧 郝云彬[3] 张小军 梅光明 陈思 严忠雍 李佩佩 常家琪 韩程程 

机构地区：[1]浙江海洋大学水产学院,浙江舟山316022 [2]浙江海洋大学海洋与渔业研究所浙江省海洋水产研究所,浙江舟山316021 [3]江南大学食品学院,江苏无锡214122 [4]浙江海洋大学食品与医药学院,浙江舟山316022

出　　处：《浙江海洋大学学报（自然科学版）》2017年第6期511-515,共5页Journal of Zhejiang Ocean University：Natural Science

基　　金：杭州市社发项目(20150533B42)

摘　　要：建立一种准确测定保鲜剂样品中4-己基间苯二酚的超高效液相色谱-荧光色谱的检测方法。色谱条件为色谱柱(2.1 nm×150 mm,1.7μm),乙腈-水(70:30)为流动相,激发波长280 nm,发射波长310 nm,流速为0.3 m L/min,柱温为35℃。样品通过乙腈提取,提取液经超声后高速离心,然后通过0.22μm有机相微孔滤膜过滤后上机进样,进行超高效液相色谱-荧光色谱分析。方法在0.10~20.00μg/m L(R=0.999)呈良好的线性关系,其回收率为83.75%~100.70%,相对标准偏差小于5.76%(n=6),检出限为2.0 mg/kg。利用本方法对市售5种保鲜剂进行了分析,发现其中一种含有4-己基间苯二酚,另外4种均为阴性样品。本方法快速、准确、灵敏度高,可广泛用于保鲜剂中4-己基间苯二酚含量的分析测定。A method for the determination of 4-hexylresorcinol in the samples of aquatic preservative was established by ultra performance liquid chromatography-fluorescence spectroscopy was established （UPLC- FLD）. The chromatographic column conditions were as follows： （2.1 nm×150 mm, 1.7 μm）, acetonitrile-water （70：30） as the mobile phase. The excitation wavelength was 280 nm, the emission wavelength was 310 nm, the flow rate was 0.3 mL/min and the column temperature was 35 ℃. The sample was extracted with acetonitrile, and the extract was centrifuged at high speed after ultrasonic irradiation. Then, the supernatant were filtered through a 0.22 μm organic phase micro membrane and then injected into fluorescence spectroscopy （FLD） to analysis. The standard solution of 4-hexylresorcinol was in the range of 0.10-20.00 μg/mL （R=0.999） showed a good linear relationship, the average recoveries were 83.75%-100.70% and the relative standard deviations were less than 5.76%（n=6）, the detection limit was 2.0 mg/kg. The results showed that only one of the five kinds of preservatives contained 4-hexylresoreinol and the other four were negative samples. This method is rapid, aeeurate and sensitive, and it is suitable for determination of content in preservative.

关 键 词：超高效液相色谱 保鲜剂 4-己基间苯二酚 

分 类 号：TS254.4[轻工技术与工程—水产品加工及贮藏工程]