超高效液相色谱串联质谱法测定牛羊脂肪中三氯苯达唑及其代谢物残留量
Determination of Residues of Triclabendazole and Its Metabolite in Cattle and Sheep Fat by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
侯冰1
作者信息
- 1. 丹东市市场监管事务服务中心(丹东市检验检测认证中心),辽宁 丹东 118000
- 折叠
摘要
采用超高效液相色谱串联质谱法建立了牛、羊脂肪中三氯苯达唑及其代谢物三氯苯达唑酮残留量的测定方法.样品用乙腈提取,正己烷净化,采用BEH C18 色谱柱、乙腈-0.1%甲酸溶液梯度洗脱分离,电喷雾负离子模式测定.结果显示,三氯苯达唑和三氯苯达唑酮在 5～500 ng·mL-1 浓度范围内线性关系良好(R2＞0.99);方法检出限和定量限均为 0.5 μg·kg-1 和 1 μg·kg-1;在 1 μg·kg-1、10 μg·kg-1、50 μg·kg-1 添加水平下平均回收率在 81.6%～102.3%,批内(n=6)及批间(n=3)相对标准偏差≤14.0%.方法准确度高,精密度好,适用于牛、羊脂肪中三氯苯达唑及其代谢物残留量的测定.
Abstract
A method for the determination of residues of triclabendazole and its metabolite ketotriclabendazole in cattle and sheep fat was established using ultra performance liquid chromatography-tandem mass spectrometry.The sample was extracted with acetonitrile,purified with hexane,separated by BEH C18 chromatographic column,gradient elution with acetonitrile and 0.1%formic acid solution,and determined by electrospray negative ion mode.The results showed that there was a good linear relationship(R2＞0.99)between triclabendazole and ketotriclabendazole in the range of 5～500 ng·mL-1;the detection limit and quantification limit of the method were both 0.5 μg·kg-1 and 1 μ g·kg-1;the average recoveries were between 81.6%and 102.3%at the addition levels of 1 μg·kg-1,10 μg·kg-1,and 50 μg·kg-1,and the relative standard deviations within the batch(n=6)and between batches(n=3)were≤14.0%.This method has high accuracy and good precision,which is suitable for determination of residues of triclabendazole and its metabolite in cattle and sheep fat.
关键词
牛羊脂肪/三氯苯达唑/三氯苯达唑酮/超高效液相色谱串联质谱Key words
cattle and sheep fat/triclabendazole/ketotriclabendazole/ultra performance liquid chromatography-tandem mass spectrometry引用本文复制引用
基金项目
2022年度辽宁省市场监督管理局科技计划项目(2022ZC008)
出版年
2024
NETL
NSTL
万方数据