假博路定的鉴别研究

Study on the Identification of Counterfeit BaracludeTM

目的:通过组合检验方式,识别假冒抗乙肝药物博路定。方法:以博路定为例,研究建立其外观鉴别法;采用超高效液相色谱-质谱联用技术对博路定伪品进行实验室确证,色谱柱为Agilent ZORBAX Exlend Plus C18(2.1 mm×50 mm,1.8μm),流动相为乙腈和0.02 mol·L^-1乙酸铵溶液(含0.1%甲酸),梯度洗脱,检测波长为254 nm,流速为0.3 mol·min-1,柱温为35℃。ESI离子源,正离子检测模式,离子源温度为350℃。结果:博路定真、伪品的外观存在明显差别,利用外观鉴别法初步判断其真伪。在液质联用的谱图中,博路定伪品出现与阿德福韦酯对照品色谱保留时间、一级质谱图和二级质谱图一致的色谱峰,证明博路定伪品中的主药成分为阿德福韦酯。结论:运用简便外观鉴别技术,可初步筛查可疑性假药,经液质联用验证,能有效提高药品监督的质量。

Objective: To identify counterfeit anti-hepatitis B drugs by using a combination test method.Methods: BaracludeTM was used as an example to establish an appearance identification method. The highperformance liquid chromotography-mass spectrometry was used to confirm the identification. The separation was carried out on an Agilent ZORBAX Exlend Plus C18 column(2.1 mm × 50 mm, 1.8 μm) eluted with acetonitrile and 0.02 mol·L^-1 ammonium acetate solution(containing 0.1% formic acid) in a gradient mode at a flow rate of 0.3 mL·min-1. The detection wavelength was set at 25 nm. The column temperature was set at 35 ℃. ESI ion source and positive ion detection mode were applied at 350 ℃. Results: Genuine BaracludeTMshowed obvious differences in appearance. Therefore, the appearance identification method can be used to judge the authenticity of samples. In the LC/MS spectrum of the counterfeit, the retention time,the first-order mass spectrum and the second-order mass spectrum of the chromatographic peak were the same as those of the adefovir dipivoxil reference substance. The component in the counterfeit was adefovir dipivoxil. Conclusion: The simple and convenient appearance identification can preliminarily screen suspected counterfeit drugs, which, combined with laboratory verification, can effectively improve the quality of drug supervision.