高效液相色谱串联质谱法测定饲料中8种利尿剂药物

本研究旨在建立一种高效液相色谱串联质谱法测定饲料中8种利尿剂的检测方法。样品经乙腈提取,HLB固相萃取小柱净化,氮吹浓缩,以10 mmol/L乙酸铵水溶液(含0.1%甲酸)和乙腈为流动相,C₁₈色谱柱梯度洗脱分离,采用电喷雾正、负离子源同时采集,多反应监测模式进行检测。结果表明,该方法8种化合物在(2.00～100) ng/ml的范围内均有良好的线性,相关系数r^2>0.99。添加浓度水平为(2.00～10.0)μg/kg时,平均回收率为68.7%～104.8%,相对标准偏差为2.3%～5.0%,方法检出限为(0.1～0.5)μg/kg,定量限为(0.3～1.5)μg/kg。该方法简便、快速、结果准确度高,适用于饲料中利尿剂的检测。

Determination of 8 diuretics in feed by HPLC-MS/MS

The aim of this study was to establish a high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS) method for the determination of 8 diuretics in feed.The samples were extracted with acetonitrile,purified with HLB solid phase extraction cartridges,concentrated with nitrogen at last.The analytes were separated on a C18 columm with 10 mmol/L ammonium acetate aqueous which contained 0.1% formic acid and acetonitrile as mobile phases,and finally analyzed using electrospray ionization in positive and negative ion mode with multiple reaction monitoring(MRM).The result showed that the 8 compounds in this method have good linearity in the range from 2.00 to 100 ng/ml,and the correlation coefficient is r2>0.99.When the concentration level is 2.00-10.0 μg/kg,the average recovery is 68.7%-104.8%,the relative standard deviation is 2.3%-5.0%,the detection limit is 0.1-0.5 μg/kg,the quantitative limit is 0.3-1.5 μg/kg.The method is simple,rapid and accurate and suitable for the detection of diuretic in feed.