超高效液相色谱-串联质谱法测定饲料中6大类50种药物

Simultaneous determination of 50 drugs in feeds by ultra performance liquid chromatographyelectrospray ionization tandem quadrupole mass spectrometric

建立了饲料中超高效液相色谱-串联质谱法同时测定6类药物(磺胺类、喹诺酮类、氯霉素类、四环素类、大环内酯类和受体激动剂)。样品经甲醇/水/甲酸(体积比49/49/2)提取,HLB固相萃取小柱净化,超高效液相色谱-串联质谱仪测定,ESI正负离子同时扫描,以多反应监测方式采集数据,外标法定量。50种药物在饲料基质溶液中,在10~500μg/L范围内具有良好的线性关系(r>0.99);在4个不同浓度加标水平下,各药物的平均回收率在60.4%~130%之间,RSD为1.1%~21%,方法的定量限为1~8μg/kg。经实际饲料样品确证分析,方法适用于饲料中多种药物的同时检测。

An ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric （UPLC-ESI-MS/MS） method was developed for the simultaneous determination of 50 drugs in feeds such as sulfonamides, chloramphenicols, quinolones, tetracyclines, macrolides and ^-agonists. The sample was extracted with methanol/water/formic acid （49/49/2, V/V/V）, and then cleaned up using solid phase extraction with an Oasis HLB column, detected by UPLC-ESI-MS/MS. The ESI-MS/MS detection was achieved in positive and negative modes under multiple reaction monitoring （MRM） mode. The linear ranges were from 0. 01 to 0. 5 mg/L with the correlation coeiticients above 0. 99 for all the 50 drugs. The average recoveries of the 50 drugs spiked in feeds at four spiked levels were 60. 4% ~ 130% with the relative standard deviations of 1.1% ~ 20. 7%. The limits of detection,were 1μg/kg ~ 8μg/kg. The method is rapid, accurate, reproducible and sensitive, and suitable for the simultaneous determination of diverse drugs in compound feeds.