高效液相色谱法测定水产品中喹乙醇代谢物残留量

doi:10.7506/spkx1002-6630-201310056

食品科学 ›› 2013, Vol. 34 ›› Issue (10): 255-258.doi: 10.7506/spkx1002-6630-201310056

高效液相色谱法测定水产品中喹乙醇代谢物残留量

贝亦江，王扬，何丰，任胜兰

1.浙江省水产质量检测中心，浙江杭州 310012；2.浙江科技学院生物与化学工程学院，浙江杭州 310023

收稿日期:2012-02-16 修回日期:2013-03-31 出版日期:2013-05-25 发布日期:2013-05-07
通讯作者: 贝亦江 E-mail:zsbij@163.com
基金资助:
浙江省科技厅水产品加工产业团队课题

Determination of Olaquindox Metabolite Residues in Fishery Products by High Performance Liquid Chromatography

BEI Yi-jiang，WANG Yang，HE Feng，REN Sheng-lan

1. Aquatic Product Quality Testing Center of Zhejiang Province, Hangzhou 310012, China；
2. School of Biological and Chemical Engineering, Zhejiang University of Science and Technology, Hangzhou 310023, China

Received:2012-02-16 Revised:2013-03-31 Online:2013-05-25 Published:2013-05-07
Contact: Jiang YiBei E-mail:zsbij@163.com

摘要/Abstract

摘要：

建立高效液相色谱法对水产品中喹乙醇代谢物(3-甲基喹噁啉-2-羧酸)残留量的检测方法。样品用2.0mol/L的盐酸水解，固相萃取净化，反相色谱柱分离，紫外检测器检测，外标法定量。喹乙醇代谢物在质量浓度0.01～1.0μg/mL的范围内呈线性关系，相关系数为0.9998，检出限为4.0μg/kg，定量限为12.0μg/kg。喹乙醇代谢物回收率在71.0%～86.5%之间，相对标准偏差在3.84%～7.32%之间。对样品前处理过程进行优化，增加提取步骤、缩短酸解时间后，回收率平均提高6.4%；同时发现，不过滤比过滤的回收率平均提高13.0%。

关键词: 高效液相色谱, 水产品, 喹乙醇代谢物

Abstract:

A high performance liquid chromatography method was established to determine olaquindox metabolite
(3-methyl-2-quinoxalinecarboxylic acid, MQCA) residues in fishery products in this study. Olaquindox metabolite
residues were extracted with 2 mol/L hydrochloric acid, and purified on an SPE column. Sample analysis was performed
using RP-HPLC and external standard method. In the concentration range of 0.01 to 1.0 μg/mL, an excellent linearity
was observed with a correction coefficient of 0.9998. The LOD (limit of detection) was 4.0 μg/kg and LOQ (limit of
quantification) was 12.0 μg/kg. Average recovery rates for different species of fishery products spiked at three levels
varied between 71.0% and 86.5% with a RSD of 3.84% to 7.32%. The recovery of MQCA was increased by an average
of 6.4% under optimized pretreatment conditions with more complicated extraction procedure and shortened oscillation
time. Moreover, an average increase of 13.0% in MQCA recovery was obtained by omitting filtration.

Key words: high performance liquid chromatography, fishery product, olaquindox metabolite residues

贝亦江，王扬，何丰，任胜兰. 高效液相色谱法测定水产品中喹乙醇代谢物残留量[J]. 食品科学, 2013, 34(10): 255-258.

BEI Yi-jiang，WANG Yang，HE Feng，REN Sheng-lan. Determination of Olaquindox Metabolite Residues in Fishery Products by High Performance Liquid Chromatography[J]. FOOD SCIENCE, 2013, 34(10): 255-258.

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高效液相色谱法测定水产品中喹乙醇代谢物残留量

Determination of Olaquindox Metabolite Residues in Fishery Products by High Performance Liquid Chromatography

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