现代畜牧科技2024,Issue(11) :10-12.DOI:10.19369/j.cnki.2095-9737.2024.11.004

基质分散固相萃取—高效液相色谱法检测鸡蛋中氯羟吡啶和二硝托胺药物残留

Determination of Clopidol and Dinitolmide Residues in Eggs based on Matrix Dispersion Solid-phase Extraction and High Performance Liquid Chromatography

陈芳 张文文 曾云凤 刘昨 李文静 陈宝宇 周振新 贺敏华 卜泽明
现代畜牧科技2024,Issue(11) :10-12.DOI:10.19369/j.cnki.2095-9737.2024.11.004

基质分散固相萃取—高效液相色谱法检测鸡蛋中氯羟吡啶和二硝托胺药物残留

Determination of Clopidol and Dinitolmide Residues in Eggs based on Matrix Dispersion Solid-phase Extraction and High Performance Liquid Chromatography

陈芳 1张文文 1曾云凤 1刘昨 1李文静 1陈宝宇 1周振新 1贺敏华 1卜泽明1
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作者信息

  • 1. 广西壮族自治区兽药监察所,广西 南宁 530001
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摘要

建立基于基质分散固相萃取(MSPD)—高效液相色谱法(HPLC)同步检测鸡蛋中氯羟吡啶和二硝托胺残留的快速、高效、经济的方法.鸡蛋样品经甲醇—乙腈混合溶液提取,利用200 mg十八烷基键合硅胶吸附剂(C18)和50 mg N-丙基乙二胺(PSA)混合分散固相萃取粉末净化,C18色谱柱分离,纯水—乙腈作为流动相进行梯度洗脱,外标法进行定性定量分析.结果表明,氯羟吡啶和二硝托胺在0.025~50.0 μg/mL范围呈良好的线性关系(R2>0.999),检出限为0.025 mg/kg和0.050 mg/kg,定量限为0.075 mg/kg和0.100 mg/kg.在0.1、2.5 mg/kg和5.0 mg/kg水平的加标回收试验中,氯羟吡啶的回收率为87.70%~101.78%,相对标准偏差(RSD)为0.66%~5.41%;二硝托胺的回收率为84.99%~97.11%,RSD为0.95%~5.34%.该方法简便、净化效果好、回收率高,适用于鸡蛋中氯羟吡啶和二硝托胺药物的同步定量检测.

Abstract

To establish a rapid,efficient,and cost-effective method for the simultaneous determination of clopidol and dinitolmide residues in eggs based on matrix solid-phase dispersion extraction and high performance liquid chromatography.Egg samples were extracted with a methanol-acetonitrile mixture,purified using a mixture of 200 mg octadecylsilane bonded phase and 50 mg primary secondary amine for dispersion solid-phase extraction,separated using a C18 column,and eluted with a gradient of water-acetonitrile as the mobile phase.Quantitative and qualitative analysis were conducted using an external standard method.Results show that the clopidol and dinitolmide exhibited good linear relationships in the range of 0.025~50.0 μg/mL(R2>0.999).The limits of detection were 0.025 mg/kg and 0.050 mg/kg,while the limits of quantitation were 0.075 mg/kg and 0.100 mg/kg for clopidol and dinitolmide In the spiked recovery tests at levels of 0.1,2.5 mg/kg,and 5.0 mg/kg,the recovery rates for clopidol ranged from 87.70%~101.78%,with relative standard deviations ranging from 0.66%~5.41%.For dinitolmide,the recovery rates ranged from 84.99%~97.11%with relative standard deviations ranging from 0.95%~5.34%.This method is simple,with good purification effects and high recovery rates,making it suitable for the simultaneous quantitative detection of clopidol and dinitolmide residues in eggs.

关键词

固相萃取/高效液相色谱法/药物/残留

Key words

solid phase extraction/high performance liquid chromatography/drug/residue

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出版年

2024
现代畜牧科技
黑龙江省畜牧研究所

现代畜牧科技

影响因子:0.066
ISSN:2095-9737
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