摘要
建立了高效液相色谱—串联质谱法检测中兽药注射剂中非法添加13种喹诺酮类药物的方法。样品经0.2%甲酸溶液溶解后稀释,以0.2%甲酸溶液与甲醇作为流动相进行梯度洗脱,采用多反应监测模式进行测定。13种喹诺酮类药物检测限(LOD)为0.1~0.5 ng/mL,定量限(LOQ)为1~5 mg/mL,在5.0200 ng/mL范围内线性关系良好,相关系数均大于0.99在5 mg/mL、10 mg/mL、20mg/mL三个添加浓度下,平均回收率90.9%~101.9%,相对标准偏差为0.6%~3.8%。该法准确、简单、快速。
A method of HPLC-MS/MS was developed to the determination 13 quinolones illegally added of in traditional Chinese medicine for animal.The sample was dissolved and diluted with 0.2%formic,then Separate with HPLC which was using gradient elution with methanol and 0.2%formic acid.Qualitative and quantitative analysis of the 13 quinolones were carried out in multiple reactions monitoring mode(MRM).The limits of detection(LODs) of 13 quinolones were in the range of 0.1~0.5 ng/mL.the limits of quantitation(LOQs) of 13 quinolones were in the range of 1~5 mg/ mL.The correlation coefficient of 13 quinolones ranged from 5.0 ~ 200 ng / mL was greater than 0.99.The results showed that when the concentrations of 13 quinolones were between 5 and 20 mg/mL,the average recoveries ranged from90.9%to 101.9%,with relative standard deviations of 0.6%-3.8%.The method was accurate,simple and fast.
引文
[1]农业部.中华人民共和国农业部公告第1025-14-2008号[S]
[2]温中明,李东,徐玉红.高效液相色谱法同时测定人血浆中多种喹诺酮类药物浓度[J].中国药业,2011,20(14):25-27
[3]GB/T 21312-2007动物源性食品中14种喹诺酮药物残留检测方法液相色谱-质谱/质谱法[s]
[4]李佩佩,郭远明,陈雪昌,等.色谱法检测动物源食品中喹诺酮类药物残留研究进展[J].食品科学,2013,(3):303~307
[5]中国兽药典委员会.中华人民共和国兽药典二○一○年版(一部)[s]
[6]农业部.中华人民共和国农业部公告第2508号[s]