UPLC-MS/MS法测定3种中兽药制剂中非法添加的阿莫西林和氨苄西林

Detection of Illegally Added Amoxicillin and Ampicillin in 3 Kinds of Traditional Chinese Medicine for Animals by UPLC-MS/MS

关键词:  中兽药制剂  阿莫西林  氨苄西林  超高效液相串联质谱法

Key words:  Traditional Chinese Medicine for Animals  Amoxicillin  Ampicillin  UPLC-MS/MS

摘要:

应用超高效液相色谱-串联质谱技术,建立了3种中兽药制剂中非法添加阿莫西林和氨苄西林的检测方法。样品经50 %乙腈水溶液溶解后,稀释。实验采用0.2 %甲酸乙腈溶液与0.2%甲酸水溶液作为流动相进行梯度洗脱,经Atlantis T3柱 (2.1 mm*150 mm, 5 μm)分离,通过多反应监测模式进行测定。结果表明阿莫西林和氨苄西林在1～50 ng/mL的范围内线性关系良好；阿莫西林和氨苄西林的最低检测限分别为0.2 mg/g 和0.5 mg/g；阿莫西林回收率在83.4%~95.8%之间,RSD 2.0%~4.6%,氨苄西林回收率在85.1%~97.2%,RSD为1.7%~4.0%。本方法准确、可靠,可用于中兽药制剂中非法添加阿莫西林和氨苄西林的检测。

Abstract:

A method based on ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of Amoxicillin and Ampicillin illegally added in 3 kinds of traditional Chinese medicine for animals. Samples were dissolved in 50% acetonitrile solution and diluted. The UPLC separation was performed on Atlantis T3 column with a linear gradient elution program of 0.2% formic acid acetonitrile and 0.2% formic acid aqueous solution as the mobile phase. Multiple reaction monitoring was used for the selective detection. The result demonstrated that the linearity range of Amoxicillin and Ampicillin was 1～50 ng/mL, the limit of detection of Amoxicillin and Ampicillin were 0.2 mg/g and 0.5 mg/g, respectively. The recovery was 83.4%~95.8% with RSD of 2.0%~4.6% for Amoxicillin, and the recovery was 85.1%~97.2% with RSD of 1.7%~4.0% for Ampicillin. It indicated that the method was accurate and reliable in the determination of Amoxicillin and Ampicillin illegally added in 3 kinds of traditional Chinese medicine for animals.