固相萃取-液质联用法用于乌鸡白凤丸中动物药的质量控制初探

Study on the Quality Control of Animal Ingredients in Wuji Baifeng Pills by SPE-UPLC-QQQ

目的:建立乌鸡白凤丸中鹿角胶、鹿角霜和鳖甲的鉴别和掺伪检查方法。方法:采用胰蛋白酶对乌鸡白凤丸样品酶解处理,利用固相萃取-超高效液相色谱-三重四极杆质谱(SPE-UPLC-QQQ)对样品中的鹿、鳖、猪、牛、马、驴、角鳖、佛罗里达鳖源性成分的专属性特征离子进行检测。结果:方法的专属性、精密度和灵敏度均符合分析检测的技术要求。12批样品检测到了处方中规定的鹿、鳖源性成分,部分样品也检出了处方中未规定的猪、牛源性成分。结论:所建立的方法经方法学验证,专属性强,为乌鸡白凤丸的质量控制及标准研究提供了参考。

Objective: To establish an analysis method for the identification and inspection of Cervi Cornus Colla,Cervi Cornus Degelatinatum and Trionycis Carapax in Wuji Baifeng pills. Methods: Trypsin was used to hydrolyze the samples. Solid phase extraction-ultra high performance liquid phase-triple quadrupole mass spectrometry( SPE-UPLC-QQQ) was used to detect the specific characteristic ions of horse,ox,pig,deer,Trionyx sinensis Wiegmann,Apalone spinifera,Apalone ferox( Schneider) in Wuji Baifeng pills.Results: The established present method was specific,precise and reliable. All of 12 detected samples presented the genuine ingredients specified in the prescription. Some of the samples presented the adulterant ingredients with pig and ox sources.Conclusion: The methodology validation was performed and the results were satisfied. The method provides scientific reference for the study on quality control methods for Wuji Baifeng pills.