高效液相色谱荧光法测定水产品中喹哪啶麻醉剂残留量  

Determination of quinaldine residues in aquatic products by high performance liquid chromatography with fluorescence detector

作　　者：徐闪浪 黄和 高平[4] 陈日檬 曾丹丹 陈营寿 XU Shanlang;HUANG He;GAO Ping;CHEN Rimeng;ZENG Dandan;CHEN Yingshou(Guangdong Provincial Key Laboratory of Aquatic Product Processing and Safety,Zhanjiang 524088;Key Laboratory of Advanced Processing of Aquatic Product of Guangdong Higher Education Institution,Zhanjiang 524088;College of Food Science and Technology,Guangdong Ocean University,Zhanjiang 524088;Zhanjiang Institute for Food and Dmg Control,Zhanjiang 524022)

机构地区：[1]广东省水产品加工与安全重点实验室,湛江524088 [2]水产品深加工广东普通高等学校重点实验室,湛江524088 [3]广东海洋大学食品科技学院,湛江524088 [4]湛江市食品药品检验所,湛江524022

出　　处：《分析试验室》2020年第9期1035-1039,共5页Chinese Journal of Analysis Laboratory

基　　金：“十三五”国家重点研发计划重点专项(2019YFD0901605);广东省科技计划项目(2014A02020812)资助。

摘　　要：建立了水产品中喹哪啶麻醉剂残留量的高效液相色谱荧光法检测方法。样品采用1%三氯乙酸-乙腈混合溶液提取,经混合型阳离子交换固相萃取柱净化,0.02 mol/L NH4H2PO4溶液-乙腈(65:35,V:V)为流动相,ZORBAX Eclipse XDB-C18色谱柱分离,荧光检测器,激发波长为238 nm,发射波长为417 nm,外标法定量。结果表明,喹哪啶麻醉剂在10~500μg/L范围内呈现良好线性关系,相关系数(R2)为0.9999,回收率为74.5%~100.6%,相对标准偏差为1.6%~7.5%,方法检出限(LOD)为0.015 mg/kg,定量限(LOQ)为0.050 mg/kg。该方法可满足水产品中喹哪啶麻醉剂残留分析的要求。A method for the determination of quinaldine residues in aquatic products was established by high performance liquid chromatography with fluorescence detector. The sample was extracted with a solution mixed1% trichloroacetic acid-acetonitrile,purified by solid-phase extraction column,and finally quantified by external standard method. The compound was separated on a reversed-phase ZORBAX Eclipse XDB-C18 column using 0. 02 mol/L ammonium dihydrogen phosphate solution-acetonitrile( 65: 35,V: V) as mobile phase,and detected by the fluorescence detector at an excitation wavelength of 238 nm and an emission wavelength of417 nm. The results showed that the limit of detection and the limit of qualification were 0. 015 mg/kg and0. 050 mg/kg,respectively. The calibration curves of quinaldine showed good linearity in the range of 10-500 μg/L with a high correlation coefficient of 0. 9999. The recoveries were in the range of 74. 5%-100. 6%,with the relative standard deviations( RSDs) of 1. 6%-7. 5%. This method is suitable for the quinaldine residue analysis in aquatic products.

关 键 词：高效液相色谱 水产品 喹哪啶 固相萃取 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.7[轻工技术与工程—食品科学与工程]