摘要
建立了中兽药制剂中20种氟喹诺酮类药物检测的超高效液相色谱-串联质谱方法。液相色谱条件为:色谱柱BEH C_(18)柱(100 mm×2.1 mm,1.7μm);流动相为甲醇/乙腈溶液-0.2%甲酸水溶液,梯度洗脱;柱温40℃;流速0.2 mL/min;进样量5μL。质谱条件为:电喷雾离子源(ESI+),多反应监测(MRM)方式采集,外标法定量。试验结果表明,20种FQs药物在25～500 ng/mL浓度范围内呈现良好线性关系,相关系数R^2均大于0.995;方法检测限为5μg/g;从5、1 0和20 mg/g三个添加浓度检测结果可以看出,方法平均回收率为80.3%～11 2.9%(n=6),批内批间RSD均小于10%。
A UPLC-MS/MS method was established for the determination of 20 Fluoroquinolones in traditional Chinese medicine powders.UPLC condition:the chromatography column BEH C_(18) column of 100 mm×2.1 mm,1.7μm;mobile phase is methanol/acetonitrile and water(0.2%formic acid);column temperature is 40℃;flow rate is 0.2 mL/min;injection volume is 5μL.Mass spectrometry condition:ESI+ and MRM mode.The calibration curve was good linear between 25～500ng/mL,R2 was greater than 0.995.The limit of detection of the method was 5μg/g;The average recoveries at the three concentrations of 5、10 and 20 mg/g ranged from 80.3%to 112.9%(n=6),intra- and inter-batch variation coefficients were less than 10%.
出处
《现代畜牧兽医》
2013年第6期40-42,共3页
Modern Journal of Animal Husbandry and Veterinary Medicine
