Yan Lijuan, Zhang Feng, Fang Enhua, Guo Yanni, Zhou Yu, Lin Liyi, Chu Xiaogang
Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361012, China.
Se Pu. 2010 Nov;28(11):1038-42.
A method for the simultaneous determination of six macrolide antibiotics (oleandomycin, erythromycin, kitasamycin, josamycin, roxithromycin and tylosin) and two lincosamide antibiotics (lincomycin and clindamycin) in animal feeds by ultra-performance liquid chromatography-electrospary ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed. The macrolide and lincosamide antibiotics were extracted from the feeds with methanol followed by enrichment and clean-up with an Oasis HLB cartridge. The UPLC separation was performed on a Waters Acquity UPLC BEH C18 column by a gradient elution using 0.1% formic acid and acetonitrile as the mobile phase at a flow rate of 0.3 mL/min. The identification of eight drugs was carried out by positive electrospray ionization in multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 1-100 microg/L. The average recoveries of the eight drugs from the feeds spiked at 1, 10 and 100 microg/kg levels were between 68.6% and 95.2%, and the relative standard deviations (RSD) were between 4.9% and 11.8%. The limits of quantification (LOQ) of the drugs in the feeds were 1 microg/kg. The method is simple, rapid, sensitive and suitable for the simultaneous determination of macrolide and lincosamide antibiotics in animal feeds.
建立了一种超高效液相色谱-电喷雾电离串联质谱法（UPLC-ESI-MS/MS）同时测定动物饲料中六种大环内酯类抗生素（竹桃霉素、红霉素、吉他霉素、交沙霉素、罗红霉素和泰乐菌素）和两种林可酰胺类抗生素（林可霉素和克林霉素）的方法。大环内酯类和林可酰胺类抗生素用甲醇从饲料中提取，然后用Oasis HLB柱进行富集和净化。UPLC分离在Waters Acquity UPLC BEH C18柱上进行，采用梯度洗脱，以0.1%甲酸和乙腈为流动相，流速为0.3 mL/min。八种药物的鉴定采用正电喷雾电离在多反应监测（MRM）模式下进行，定量分析采用外标法。校准曲线在1-100 μg/L范围内线性良好。在添加水平为1、10和100 μg/kg的饲料中，八种药物的平均回收率在68.6%至95.2%之间，相对标准偏差（RSD）在4.9%至11.8%之间。饲料中药物的定量限（LOQ）为1 μg/kg。该方法简便、快速、灵敏，适用于同时测定动物饲料中的大环内酯类和林可酰胺类抗生素。
