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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,5?m),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 m L·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8.89~1 066.7、9.70~1 789.5、10.90~2 179.6、9.70~1 940.3、9.53~3 810.2和9.87~3 948.0 ng,r2分别为0.999 7、0.999 5、0.999 9、1.000 0、1.000 0和1.000 0;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 establish a HPLC method for the simultaneous determination of 6 components in magnoliaceae, cork hydrochloride, berberine, schisandrin, schisandrin and schisandrin in Gynecological Tablets. METHODS: The mobile phase was eluted with a Waters Symmetry C18 column (250 mm × 4.6 mm, 5 μm) using acetonitrile and 0.033 mol·L -1 potassium dihydrogen phosphate as mobile phase at a flow rate of 0.8 m L · min -1 , Detection wavelength 220 nm. Results: The six chemical components showed good resolution and no negative interference. The average recoveries (n = 6) ranged from 97.5% to 108.0% (RSD 1.6% -2.8%). Repeated RSD (n = 6) Was 1.5% -3.3%. The linear ranges of magnolol, cork base, berberine, schisandrin, schizandrin B and Schisandrin B were 8.89-1.0667, 9.70-1789.5 and 10.90-2 179.6 , 9.70 ~ 1 940.3, 9.53 ~ 3 810.2 and 9.87 ~ 3 948.0 ng, r2 respectively 0.999 7,0.999 5,0.999 9,1.000 0,1.000 0 and 1.000 0; the components of the test solution are stable within 24 h. The contents of six components of magnolol, cork hydrochloride, berberine, schisandrin, schisandrin B and Schisandrin B in 8 batches of samples were 0.183 ~ 0.282, 0.674 ~ 2.313, 11.540 ~ 18.010, 0.045 ~ 0.659, 0.006 ~ 0.110 and 0.004 ~ 0.343 mg · g-1. Conclusion: The newly established method is validated by methodology, which can effectively control the quality of Gynecology girdle strip and can also be used as a new method to improve the new content of the standard.