康寿丸质量标准提升研究

Improvement of the Quality Standard of Kangshou Pills

目的提升康寿丸的质量标准。方法采用薄层色谱(TLC)法对康寿丸中的人参、地骨皮、何首乌进行定性鉴别;采用高效液相色谱法测定制剂中2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷(简称二苯乙烯苷)的含量,色谱柱为Phenomenex C18柱(250 mm×4.6 mm,4µm),流动相为乙腈-水(19∶81,V/V),流速为1.0 mL/min,检测波长为320 nm,柱温为25℃,进样量为10µL。测定2家生产厂家各10批样品中二苯乙烯苷的含量,并制订其含量限度。结果人参、地骨皮和何首乌的薄层色谱图主斑点清晰,分离度良好,且阴性对照无干扰。二苯乙烯苷的进样量在30.094~3761.7 ng范围内与峰面积积分值线性关系良好(r=1.000,n=11);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率为102.88%,RSD为0.59%(n=8)。10批样品中二苯乙烯苷含量介于1.14~3.32 mg/g。结论所建立的方法专属性强、重复性好、准确度高,可用于康寿丸的质量控制。暂订每1 g寿康丸含何首乌以二苯乙烯苷计不得少于0.90 mg。

Objective To improve the quality standard of Kangshou Pills.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify Ginseng Radix et Rhizome,Lycii Cortex,Polygoni Multiflori Radix in Kangshou Pills.High-performance liquid chromatography(HPLC)method was used to determine the content of 2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside(referred to as stilbene glycoside)in Kangshou Pills.The chromatographic column was Phenomenex C18 column(250 mm×4.6 mm,4µm),the mobile phase was acetonitrile-purified water(19∶81,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 320 nm,the column temperature was 25℃,and the injection volume was 10µL.The content of stilbene glycoside in 10 batches of samples from two manufacturers was determined and the content limit was established.Results The TLC chromatograms of Ginseng Radix et Rhizome,Lycii Cortex and Polygoni Multiflori Radix showed clear spots,good separation,and no interference from the negative control.The linear range of stilbene glycoside was 30.094-3761.7 ng(r=1.000,n=11).The RSDs of precision,stability,and repeatability test results were all lower than 2.0%,and the average recovery of stilbene glycoside was 102.88%with an RSD of 0.59%(n=8).The content of stilbene glycoside in 10 batches of samples was 1.14-3.32 mg/g.Conclusion The established method has strong specificity,good repeatability,and high accuracy,which can be used for quality control of Kangshou Pills.Temporarily,every 1 g of Kangshou Pills should contain no lower than 0.90 mg of Polygoni Multiflori Radix(calculated as stilbene glycoside).