摘要
目的:建立一种固相萃取结合高效液相色谱-串联质谱快速测定禽蛋中甲硝唑、洛硝哒唑、替硝唑、奥硝唑和二甲硝唑残留的分析方法。方法:禽蛋样品经5%三氯乙酸溶液涡旋提取、MCX固相萃取小柱净化,采用ACQUITYUPLC^(TM)BEH C_(18)色谱柱作为分析柱,采用0.1%甲酸水-甲醇作为流动相体系,采用正离子喷雾模式电离、多反应离子监测方式进行分析。结果:在0.5~50.0 ng/mL的线性范围内,5种硝基咪唑类药物的线性方程均呈良好线性关系,相关系数r^(2)>0.9984。5种硝基咪唑类药物的检出限低至0.25μg/kg,在低、中、高三组质量浓度水平下,平均加标回收率在70.8%~111.3%范围内,相对标准偏差在1.4%~6.2%范围内。结论:该方法有机试剂消耗少、低毒环保、前处理简单易操作、分析速度快、灵敏度和准确度较高,重现性好,适用于禽蛋中硝基咪唑类药物残留的检测分析。
(Objective)To establish a rapid method for the determination of metronidazole,Lonidazole,tinidazole,ornidazole and dimetronidazole residues in poultry eggs by solid phase extraction combined with high performance liquid chromatography and tandem mass spectrometry.(Methods)The egg samples were extracted by 5%trichloroacetic acid solution and purified by MCX solid phase extraction column.ACQUITY UPLC^(TM) BEH C_(18)column was used as analysis column as well as 0.1%formic acid water-methanol was used as mobile phase system.Positive ion spray mode ionization and multiple reactive ion monitoring were used for analysis.(Results)In the linear range of 0.5-50.0 ng/mL,the linear equations of the five nitroimidazole drugs showed a good linear relationship with the determination coefficient r^(2)>0.9984.The detection limits of the five nitroimidazole drugs were as low as 0.25μg/kg.The average recoveries were in the range of 70.8%to 111.3%and the relative standard deviations were in the range of 1.4%to 6.2%at the low,medium and high concentrationlevels.(Conclusion)The method is suitable for the determination of nitroimidazole residues in poultry eggs with the advantage of low consumption of organic reagents,low toxicity and environmental protection,simple pretreatment and easy operation,high analytical speed,high sensitivity and accuracy,and good reproducibility.
作者
欧阳小艳
黄珊
蒙德军
韦卓才
覃沛
Ouyang Xiaoyan;Huang Shan;Meng Dejun;Wei Zhuocai;Qin Pei(Nanning Municipal Center For Disease Control and Prevention,Nanning 530001,China;Guangxi Research Institute of Chemical Industry,Nanning 530001,China)
出处
《云南化工》
CAS
2024年第7期90-93,108,共5页
Yunnan Chemical Technology
基金
广西壮族自治区卫生健康委员会自筹科研项目(Z-A20221263)。
关键词
硝基咪唑类药物
固相萃取
高效液相色谱-串联质谱法
禽蛋
Nitroimidazole
Solid Phase Extraction
High-performance Liquid Chromatography-tandem Mass Spectrometry
Poultry Eggs
