HPLC法测定消渴降糖胶囊中槲皮素的含量(1)
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[摘要] 目的：探讨用高效液相色谱法检测消渴降糖胶囊中槲皮素的含量。方法：应用高效液相色谱法，采用C18柱，以甲醇-0.4%磷酸(55∶45)为流动相，以360 nm为检测波长，检测消渴降糖胶囊中槲皮素的含量。结果：槲皮素峰与相邻色谱峰能有效分离，柱效较高，槲皮素对照品进样量在0.056～0.560 μg范围内与峰面积呈良好的线性相关，回归方程为Y=40 103.2X-561.4，相关系数r值为0.999 8；精密度RSD=0.9%；10 h稳定性试验RSD=1.10%；重复性试验结果显示，5份样品含量的变异系数RSD=1.30%；3个不同浓度的加样回收试验，平均回收率为98.7%，RSD=0.90%。结论：采用高效液相色谱法测定消渴降糖胶囊中槲皮素的含量，专属性强，结果可靠，重现性好，可用于消渴降糖胶囊中槲皮素的含量测定。
[关键词] 高效液相色谱法；消渴降糖胶囊；槲皮素
[中图分类号] R927.2 [文献标识码] A [文章编号] 1673-7210(2011)11(a)-078-03
Determination of quercetin in Xiaoke Jiangtang Capsule by HPLC
FU Qianxia
Gong′an Health School in Jingzhou City, Hubei Province, Jingzhou 434300, China
[Abstract] Objective: To explore the method of high performance liquid chromatography (HPLC) in the determination of quercetin in Xiaoke Jiangtang Capsule. Methods: High performance liquid chromatography was employed to test the quercetin contents of Xiaoke Jiangtang Capsules. C18 column, mobile phase of methanol-0.4% phosphoric acid (55∶45) and detection wavelength of 360 nm were adopted. Results: The peak of quercetin and the adjacent peaks could be differentiated with high column efficiency. The quercetin reference standard sample size of 0.056 to 0.560 μg had a good linear correlation with the regression equation of Y=40 103.2X-561.4 and peak area (r=0.999 8), the precision RSD was 0.9% and the RSD of 10 hours stability test result was 1.10%. In repeated tests, the RSD of coefficient of variation among the 5 samples content was 1.30%; added sample tests of 3 different concentrations had average recovery rate of 98.7% and RSD was 0.90%. Conclusion: It can be concluded that, HPLC is stable and reliable in the determination of quercetin in Xiaoke Jiangtang Capsule.
[Key words] High performance liquid chromatography; Xiaoke Jiangtang Capsule; Quercetin
消渴降糖胶囊为《部颁标准》中药成方制剂第十五册收载品种，其标准号为WS3-B-2983-98。该质量标准颁布于1998年，仅涉及番石榴叶中所含槲皮素的薄层鉴别，无含量测定项目。为了更有效地控制产品质量，笔者在消渴降糖胶囊的质量标准中增加了槲皮素含量测定项目，以便对药品质量进行定性鉴别和定量测定双重控制，更有效地保证消渴降糖胶囊的内在质量。本研究旨在探讨高效液相色谱法检测消渴降糖胶囊中槲皮素含量的可靠性。
1 仪器与试药
1.1 仪器
高效液相色谱仪(P 3000型色谱泵，UV 3000型紫外检测器)；SK 8200H超声波仪(上海科导超声仪器有限公司，500 W，59 kHz)；色谱柱(KNAUER Eurospher 100，C18，5 μm，4.6 mm × 250 mm)；甲醇为色谱纯，磷酸为分析纯，水为重蒸溜水。
1.2 药品
槲皮素对照品(购于中国药品生物制品检定所，批号：0081-9304，供含量测定用)，消渴降糖胶囊样品(荆州金海药业有限公司) ......
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