HPLC法同时测定妇科止带片中6种成分的含量

目的:建立HPLC法同时测定妇科止带片中木兰花碱、盐酸黄柏碱、盐酸小檗碱、五味子醇甲、五味子醇乙、五味子乙素6种成分的含量。方法:采用Waters Symmetry^® C₁₈色谱柱(250 mm×4.6 mm,5μm),以乙腈与0.033 mol·L^-1磷酸二氢钾水溶液为流动相,梯度洗脱,流速0.8 mL·min^-1,检测波长220 nm。结果:6种化学成分分离度良好,阴性无干扰,其平均加样回收率(n=6)范围为97.5%~108.0%(RSD为1.6%~2.8%);重复性RSD(n=6)为1.5%~3.3%;木兰花碱、盐酸黄柏碱、盐酸小檗碱、五味子醇甲、五味子醇乙、五味子乙素的线性范围分别为8.89~1066.7、9.70~1789.5、10.90~2179.6、9.70~1940.3、9.53~3810.2和9.87~3948.0 ng,r²分别为0.9997、0.9995、0.9999、1.0000、1.0000和1.0000;供试品溶液各成分在24 h内稳定。8批样品中木兰花碱、盐酸黄柏碱、盐酸小檗碱、五味子醇甲、五味子醇乙、五味子乙素6个成分的含量测定结果分别为0.183~0.282、0.674~2.313、11.540~18.010、0.045~0.659、0.006~0.110和0.004~0.343 mg·g^-1。结论:新建立的方法经方法学验证,可有效控制妇科止带片的质量,也可作为提高标准中新的含量测定方法。

Objective: To develop a method for simultaneous determination of six constituents(magnoflorine, phellodendrine hydrochloride, berberine hydrochloride, schizandrin A, schisandrol B, γ-schisandrin) in Fukezhidai tablets.Methods: An HPLC method was adopted for the analysis using a Waters Symmetry^® C₁₈ column(250 mm×4.6 mm, 5 μm) with the mobile phase of acetonitrile and monopotassium phosphate in a gradient elution.The flow rate was 0.8 mL·min^-1, and the detection wavelength was 220 nm.Results: The six analytes were separated perfectly by chromatography without disturbing peaks from negative samples.Their average recoveries were 97.5%-108.0%(RSD 1.6%-2.8%, n=6), the repeatability was expressed by RSD with values of 1.5%-3.3%(n=6), and linearity ranges of magnoflorine, phellodendrine hydrochloride, berberine hydrochloride, schizandrin A, schisandrol and γ-schisandrin were respectively 8.89-1 066.7 ng(r²=0.999 7), 9.70-1 789.5 ng (r²=0.999 5), 10.90-2 179.6 ng(r²=0.999 9), 9.70-1 940.3 ng(r²=1.000 0), 9.53-3 810.2 ng(r²=1.000 0), and 9.87-3 948.0 ng(r²=1.000 0).The six analytes were stable in the sample solution within 24 h.The contents in 8 samples were in the ranges of 0.183-0.282 mg·g^-1 for magnoflorine, 0.674-2.313 mg·g^-1 for phellodendrine hydrochloride, 11.540-18.010 mg·g^-1 for berberine hydrochloride, 0.045-0.659 mg·g^-1 for schizandrin A, 0.006-0.110 mg·g^-1 for schisandrol, and 0.004-0.343 mg·g^-1 for γ-schisandrin.Conclusion: The developed method can effectively control the quality of Fukezhidai tablets, which can be used as a new assay method in the quality standard.