摘要
建立QuEChERS结合高效液相色谱串联质谱法测定饲料中氯霉素方法。样品经水相分散后用乙腈提取,经QuEChERS方法净化后,采用高效液相色谱串联质谱法测定,外标法定量。以超纯水和甲醇作为流动相,用Hypersil GOLD C18色谱柱(1.9μm,2.1 mm×100 mm)进行梯度洗脱,采用电喷雾离子源(ESI-)、负离子扫描多反应监测(MRM)模式进行定性和定量分析。结果表明:氯霉素在5.0~200.0 ng·mL^(-1)的范围内线性关系良好(r=0.9992)。在10.0、20.0、50.0μg·kg^(-1)添加水平下的回收率为84.2%~89.7%,相对标准偏差(n=6)为6.5%~8.8%,检出限(以信噪比>3计)为0.2μg·kg^(-1),定量限(以信噪比>10计)为0.6μg·kg^(-1)。该方法精密度好,灵敏度高,能简便地准确测定饲料中的氯霉素。
This study aimed to establish a method for the determination of chloramphenicol in feed by using QuEChERS combined with the high performance liquid chromatography-tandem mass spectrometry method.After water dispersion,the samples were extracted with acetonitrile.And then after the purification by QuEChERS method,the samples were determined by high performance liquid chromatography-tandem mass spectrometry and quantified by external standard method.By using the ultrapure water and methyl alcohol as mobile phases,the gradient elution was carried out by Hypersil GOLD C18 column(1.9μm,2.1 mm×100 mm).And then the qualitative and quantitative analysis was carried out by using the electrospray ionization(ESI-)and anion scanning multiple reaction monitoring(MRM)modes.The results showed that the linear relation of chloramphenicol was good in the range of 5.0-200.0 ng·mL^(-1)(r=0.9992).The recoveries at the adding levels of 10.0,20.0 and 50.0μg·kg^(-1) ranged from 84.2%to 89.7%,the relative standard deviations(n=6)were 6.5%-8.8%,the limits of detection(based on S/N>3)were 0.2μg·kg^(-1),and the limits of quantitation(based on S/N>10)were 0.6μg·kg^(-1).The method had good precision,high sensitivity and could be used to determine the chloramphenicol in feed simply and accurately.
作者
陈其煌
CHEN Qi-huang(Xiamen Agricultural Product Quality and Safety Inspection and Testing Center,Xiamen,Fujian 361009,China)
出处
《福建农业科技》
CAS
2021年第3期46-52,共7页
Fujian Agricultural Science and Technology
关键词
QUECHERS
高效液相色谱串联质谱法
氯霉素
饲料
QuEChERS
High performance liquid chromatography-tandem mass spectrometry
Chloramphenicol
Feed
