世界中医药

目的：通过高效液相色谱法测定知柏地黄丸中有效成分马钱苷及菝葜皂苷元的含量。方法：选取高效液相色谱法对知柏地黄丸中成分的含量进行测定。色谱条件采用C18色谱柱（型号为Eclipse XDB），该色谱柱的长度为250 mm，色谱柱内经为46 mm，色谱柱填料颗粒直径为5 μm。进样量为20 μL，流动相采用乙腈（A相）和01%磷酸水溶液（B相）的二元体系进行梯度洗脱。高效液相色谱法（HPLC）严谨性考察，包括线性关系、精密度、重复性、稳定性和加样回收试验考察，结果：阴性对照品溶液1在与马钱苷对照品溶液和供试品溶液色谱图相同时间处未见相同色谱峰；阴性对照品2在与菝葜皂苷元对照品溶液和供试品溶液色谱图相同时间处未见相同色谱峰。线性考察结果显示回归方程、相关系数和线性范围分别是：马钱苷在0040 54～4054 μg范围内与峰面积呈良好的线性关系，其回归方程为Y=61116X+5 6641(r=0999 7)；菝葜皂苷元进样量在0440 01～4353 μg范围内与峰面积积分值呈良好的线性关系，回归方程Y＝1639 7X+11549（r＝0999 8）。精密度试验：RSD＝079％；稳定性试验：色谱峰相对峰面积RSD平均值1716%；重复性试验：色谱峰相对峰面积RSD平均值2011%。马钱苷对照品溶液、菝葜皂苷元对照品溶液平均回收率分别为105719%、98865%，RSD分别为129%、136%。201805026、201806013、201807085等3个不同批次号的知柏地黄丸中，马钱苷成分和菝葜皂苷元成分的含量差异无统计学意义。结论：高效液相色谱法的操作简单，结果具有较好的精密度、稳定性和重复性，可作为知柏地黄丸质量控制的有效方法，而不同批次知柏地黄丸中有效成分含量未见明显差异。

English Summary:

To determine the content of loganin and sarsasapogenin in Zhibai Dihuang Pills by HPLC.Methods:The chromatographic conditions were determined by C18 column(type Eclipse XDB).The length of the column was 250 mm，the diameter of the packing particles in the column was 5 micron，and the inner diameter of the column was 46 mm.A binary system of acetonitrile(A phase）and 01% phosphoric acid aqueous solution(B phase）was used for gradient elution.The method of high performance liquid chromatography(HPLC）was rigorous，including linear relationship，precision，repeatability，stability and sample recovery test.Based on the rigorous premise of HPLC，the content of Zhibai Dihuang Pills was determined.Results:1）Negative reference solution 1 did not show the same chromatographic peak at the same time as loganin reference solution and test solution，while negative reference solution 2 did not show the same chromatographic peak at the same time as sarsasapogenin reference solution and test solution.The results showed that loganin and sarsapogenin had good specificity. 2）Linear regression equation，correlation coefficient and linear range were：loganin had good linear relationship with peak area in the range of 0040 54~4054 μg，and the regression equation was Y=61116X+5 6641(r=0999 7); sarsapogenin injection was 044 ugh，and the regression equation Y=1639 7X+11549(r=0999 8）was obtained. 3）The precision test showed that the RSD was 079%.The stability test showed that the RSD average value of the relative peak area was 1716%.It indicated that the stability of Zhibai Dihuang Pills was good within 24 hours.The value was 2011%，indicating that the solution of Zhibai Dihuang Pills had good reproducibility. 4）The results showed that the average recoveries of loganin and sarsapogenin were 105719% and 98865% and RSD were 129% and 136% respectively，suggesting that the high-phase liquid phase detection method was reliable. 5）The contents of strychnine and sarsapogenin in Zhibai Dihuang Pills of different batches，such as 201805026，201806013 and 201807085，were not significantly different.Conclusion:The HPLC method is simple，accurate，stable and reproducible.It can be used as an effective method for quality control of Zhibai Dihuang Pills.There was no significant difference in the content of active ingredients in different batches of Zhibai Dihuang Pills.

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