徐占方 杨秀美 潘鹏飞

[摘要] 目的：建立反相高效液相色谱法同时测定双黄连胶囊中黄芩苷、黄芩素的含量。方法：采用Agilent Eclipse XDB-C18（250 mm×4.6 mm，5 μm）色谱柱，以甲醇-0.1%磷酸溶液为流动相梯度洗脱，检测波长为277 nm，流速为1.0 ml/min，进样量为10 μl，柱温为30℃。结果：黄芩苷在6.072～151.800 μg/ml范围内有良好的线性关系，r=1.000 0（n=7）；黄芩素在2.124～53.100 μg/ml范围内有良好的线性关系，r=0.999 4（n=7）。黄芩苷的平均回收率为99.21%，RSD为0.5%（n=6）；黄芩素的平均回收率为99.12%，RSD为0.6%（n=6）。结论：本法操作简便、快速、结果准确，可用于双黄连胶囊的质量控制。

[关键词] 含量测定；黄芩苷；黄芩素；高效液相色谱法

[中图分类号] R927.2 [文献标识码] A[文章编号]1673-7210（2011）11（c）-067-03

Simultaneous determination of contents of Baicalin and Baicalein in Shuanghuanglian Capsules by high performance liquid chromatography

XU Zhanfang1, YANG Xiumei2, PAN Pengfei1

1.Jixi Food and Drug Control and Detection Center in Heilongjiang Province, Jixi 158100, China; 2.Department of Nursing, Jiguan District Hospital in Jixi City, Heilongjiaing Province, Jixi 158100, China

[Abstract] Objective: To establish simultaneous determination of the contents of Baicalin and Baicalein in Shuanghuanglian Capsules by high performance liquid chromatography (HPLC). Methods: With methanol-0.1% phosphoric acid solution as the mobile phase gradient elution, the Agilent Eclipse XDB-C18 (250 mm×4.6 mm, 5 μm) chromatographic column was used; the detection wavelength was 277 nm; the flow rate was 1.0 ml/min; the injection volume was 10 μl; the column temperature was 30℃. Results: The Baicalin showed a favorable linear relationship in the range of 6.072-151.800 μg/ml, r=1.000 0 (n=7), while the Baicalein showed a favorable linear relationship in the range of 2.124-53.100 μg/ml, r=0.999 4 (n=7). The average recovery rate of Baicalin was 99.21%, with the relative standard deviation (RSD) was 0.5% (n=6), while the average recovery rate of Baicalein was 99.12%, with the RSD was 0.6% (n=6). Conclusion: This method is simple, fast and accurate, therefore it can be used for the quality control of Shuanghuanglian capsules.

[Key words] Content determination; Baicalin; Baicalein; High performance liquid chromatography

双黄连胶囊由金银花、黄芩和连翘三味中药组成，具有辛凉解表、清热解毒之功效，可用于发热、咳嗽、咽痛等[1]。黄芩的主要成分有黄芩苷、黄芩素、汉黄芩素[2]，双黄连胶囊中黄芩苷的HPLC法测定[3]已有报道，现行质量标准仅有黄芩中黄芩苷的定量检测，然而黄芩苷在内源酶催化水解作用下，产生大量的黄芩素[4]，仅以黄芩苷一个指标不能全面评价黄芩的质量。本文同时测定双黄连胶囊中黄芩苷、黄芩素2种主要成分的含量，结果表明，供试品在高效液相色谱中分离效果好，阴性样品溶液对测定无干扰，方法简单、准确、重复性好，可用于双黄连胶囊中黄芩的质量控制。

1 仪器与试药

HP1100高效液相色谱仪Agilent 1200LC工作站，METTLER TOLEDO电子天平AG285，KQ-400KDE型高功率数控超声波清洗器，SHIMADZU UV-2550紫外可见分光光度计；黄芩苷对照品（批号：110715-200815，含量为95.2%，中国药品生物制品检定所），黄芩素对照品（批号：111595-200604，中国药品生物制品检定所），双黄连胶囊（市售样品3批，批号：110101、091212、100701），其他试剂均为色谱纯。……