摘要
目的:建立掺伪检验方法分析逍遥丸指纹图谱。方法:首先淹没逍遥丸制成粉末待用,试验相关的混合对照品溶液和供试品溶液,通过专属性试验、线性关系分析、精密度、重复性和稳定性试验以及加样回收率试验考察逍遥丸指纹图谱方法的严谨性,采用气相色谱法(GC法)和气相色谱法-质谱法联用法(GC-MS法)检测样品中薄荷脑和香芹酮的含量,并建立掺伪检验方法。结果:专属性、线性关系、精密度、重复性和稳定性和加样回收率试验结果均显示良好。A厂逍遥丸供试品中未检出香芹酮,而B、C厂均检测出含有香芹酮,且C厂香芹酮PA值高于B厂。薄荷脑和香芹酮的GC-MS特征离子峰分别是m/z 41、55、71、81、95和m/z 39、54、82、93、108。结论:基于建立掺伪检验方法对逍遥丸进行指纹图谱检测,可有效控制其药物质量。
Objective:To study the fingerprint of Xiaoyao Pill on the basis of adulteration test method.Methods:Powder of Xiaoyao Pill was submerged for prepartion,and mixed control solution and the test solution was prepared.The precise of Xiaoyao Pill fingerprint method was tested through the specificity test,linear correlation analysis,precision,repeatability and stability test and recovery test.The menthol and carvone in the sample was tested by gas chromatography(GC),gas chromatography-mass spectrometry(GC-MS),and adulteration detection method was established.Results:1)The test results of specificity,linearity,precision,repeatability,stability and sample recovery were all good.2)Carvone was not detected in samples of Xiaoyao Pill from A factory,and detected in the samples from B and C factory.PA of carvone in samples from C factory was higher than that of B factory.3)According to GC-MS chromatogram,the results showed that GC-MS characteristic peaks of menthol and carvone were m/z 41,55,71,81,95 and 39 m/z,54,82,93,108 using positive ion mode.Conclusion:The fingerprint detection of Xiaoyao Pill on the basis of adulteration test method can effectively control drug quality.
作者
姚立山
郝满霞
Yao Lishan;Hao Manxia(Chinese Medicine Department,Nanyang Central Hospital,Affiliated Hospital of Zhengzhou University,Zhengzhou 473009,China)
出处
《世界中医药》
CAS
2018年第12期3190-3194,共5页
World Chinese Medicine
基金
河南省卫生厅2015年卫生政策研究课题(YWZY2015321)
关键词
逍遥丸
指纹图谱
掺伪检验
气相色谱法
质谱法
线性关系
专属性试验
稳定性试验
Xiaoyao Pill
Fingerprint
Adulteration Test
Gas Chromatography
Mass spectrometry
Linear relationship analysis
Specificity test
Stability test
