高效液相色谱仪——二级管阵列测器-柱前衍生法测定水产品中甲醛  

Determination of Formaldehyde in Aquatic Products by High Performance Liquid Chromatography With A Photo-diode Array Detector and Precolumn Derivation

作　　者：王志强[1] WANG Zhiqiang(Anyang Center for Disease Control and Prevention,Anyang 455000,Henan Province,China)

机构地区：[1]安阳市疾病预防控制中心

出　　处：《预防医学情报杂志》2018年第12期1548-1551,共4页Journal of Preventive Medicine Information

摘　　要：目的 建立水产品中甲醛的高效液相色谱仪——二级管阵列测器-柱前衍生检测方法。方法 试样经涡旋提取后,加入2,4-二硝基苯肼60℃水浴衍生20 min。分3次用二氯甲烷萃取,萃取液氮吹至近干,加入1 ml甲醇,过0. 22μm滤膜后进样。以甲醇-水（70＋30）为流动相,流速1. 0 ml/min,高效液相色谱仪-二级管阵列测器进行检测。结果 在0～20μg/ml浓度范围内,标准曲线线性关系良好,相关系数r〉 0. 999 0,相对标准偏差在0. 5%～5. 0%之间,加标回收率为85. 00%～99. 16%。结论 该方法样品前处理简单、快速,回收率高,准确度好,适用于水产品中甲醛含量的测定且利用二级管阵列测器检测,根据标准物质出峰保留时间和衍生物紫外吸收光谱峰定性,更有利于假阳性的判定。Objective To establish a method for the determination of formaldehyde in aquatic products by high performance liquid chromatography with a diode array detector and precolumn derivation. Methods Following vortex of the test sample, 2, 4 - dinitrophenylhydrazine was added and derivation was allowed to occur in a 60 ℃ water bath for 20 min. The derivation product was extracted three times in portion with dichloromethane, and the extraction solution was blown to near dryness using nitrogen, followed by addition of 1 ml of methanol. The resulting solution was filtered through a 0.22 Ixm membrane and injected for analysis on a high performance liquid chromatograph equipped with a photo -diode array detector using methanol -water （70 ＋ 30） as the mobile phase at a flow rate of 1.0 ml/min. Results Over 0 - 20 μg/ml, the linear relationship was good, the correlation coefficient was above 0. 999, the relative standard deviation was 0. 5% - 5.0%, and the recovery was 85.00% - 99.16 %. Conclusion With simple and rapid pretreatment, high recovery and good accuracy, this method is suitable for the determination of formaldehyde in aquatic products. Additionally, the sample is analyzed using a photo - diode array detector and identified by retention time and ultraviolet absorption spectrum of the derivation product, so false positive results can be ruled out.

关 键 词：水产品 甲醛 高效液相色谱 二级管阵列测器(PDA) 

分 类 号：TS202[轻工技术与工程—食品科学]