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目的:采用反相高效液相色谱法分别测定中药延胡索生品与醋制品中四氢非洲防己碱、原阿片碱、延胡索乙素、黄连碱、巴马汀、小檗碱、去氢延胡索甲素7个生物碱的含量,并对其进行比较。方法:采用Benetnach C18色谱柱(4.6 mm×250mm,5μm),以乙腈-0.1%磷酸水溶液(含0.08%三乙胺)为流动相,梯度洗脱,流速1.0 m L·min-1,柱温35℃,检测波长280nm,洗脱时间为70 min。结果:四氢非洲防己碱、原阿片碱、延胡索乙素、黄连碱、巴马汀、小檗碱、去氢延胡索甲素7个生物碱线性范围分别为1.12~56.0、1.27~63.5、3.37~168.5、1.02~51.0、0.89~44.5、0.88~44.0、3.22~161.0μg·m L-1(r≥0.999 3);平均回收率(n=6)为98.3%~103.6%,RSD≤2.8%。炮制前后7个生物碱含量的质量分数测定结果分别为163.90~376.28、140.24~207.29、973.61~1 158.33、180.49~433.49、68.01~196.76、18.43~46.10、550.57~1 489.84μg·g-1。结论:醋制品中四氢非洲防己碱比生品含量低,原阿片碱、延胡索乙素、巴马汀、小檗碱、去氢延胡索甲素含量均有不同程度的升高,黄连碱含量变化不定。本实验所建立方法经方法学验证,可为延胡索醋制品的质量控制提供科学依据。
OBJECTIVE: To determine the contents of tetrandrine, protopine, tetrahydropalmatine, berberine, palmatine, berberine, dehydro-fumaricin A in Chinese prodrugs and vinegar products by reversed-phase high performance liquid chromatography 7 alkaloids, and compare them. Methods: A Benetnach C18 column (4.6 mm × 250 mm, 5 μm) was used with a mobile phase of acetonitrile-0.1% phosphoric acid (containing 0.08% triethylamine) as the mobile phase at a flow rate of 1.0 mL · min -1 35 ℃, detection wavelength 280nm, elution time was 70 min. Results: The linear range of tetrakistriphenhydrylamine, protopine, tetrahydropalmatine, berberine, palmatine, berberine, and hydrogenated tetrahydropalmatine was 1.12 ~ 56.0, 1.27 ~ 63.5, 3.37 ~ 168.5,1.02 ~ 51.0,0.89 ~ 44.5,0.88 ~ 44.0,3.22 ~ 161.0μg · m L-1 (r≥0.9993). The average recoveries (n = 6) were 98.3% ~ 103.6% with RSD≤2.8%. The mass fraction of seven alkaloids before and after processing were 163.90 ~ 376.28,140.24 ~ 207.29,973.61 ~ 1 158.33,180.49 ~ 433.49,68.01 ~ 196.76,18.43 ~ 46.10,550.57 ~ 1489.84μg · g-1. CONCLUSION: Tetrahydrin in Tetrahydrofolic products in vinegar is lower than that of raw products. The contents of protopine, Tetrahydropalmatine, palmatine, berberine and Hydrochlorophilus are all increased to some extent, indefinite. The experimental method established by the methodological verification, for the quality control of corydal vinegar products provide a scientific basis.