高效液相色谱法测定消炎片中黄芩苷含量.docVIP

高效液相色谱法测定消炎片中黄芩苷含量[摘要] 目的:建立测定消炎片中黄芩苷含量的高效液相色谱法。方法:采用Diamonsil C18色谱柱(200 mm×4.6 mm,5 μm),流动相为乙腈-水-磷酸溶液(32∶68∶0.2),检测波长为280 nm,流速为1.0 ml/min,柱温为室温。结果:得回归方程为Y=114 166.67X+462 893.57,r=0.999 8(n=6), 表明进样量在0.40～2.40 μg范围内有良好的线性关系,平均回收率为(99.51±0.67)%,RSD为0.67%。结论:本方法简便、准确、重现性好,可用于消炎片的质量控制。 [关键词] 高效液相色谱法;消炎片;黄芩苷;含量测定 [中图分类号]R927.2 [文献标识码]A [文章编号]1673-7210(2009)07(a)-084-02 Content determination of baicalin in Xiaoyan Tablets by HPLC ZHAO Zhigang, LIU Xiaoli (Institute for Drug Control of Chaoyang City, Liaoning Province, Chaoyang 122000, China) [Abstract] Objective: An HPLC method for the content determination of baicalin in Xiaoyan Tablets was established. Methods: A Diamonsil C18 column(200 mm×4.6 mm, 5 μm) was used with acetonitrile-water-phosphate acid(32∶68∶0.2) as the mobile phase. The flow rate was 1.0 ml/min, the detection wavelength was 280 nm, the column temperature was room temperature. Results: The liner range was 0.40-2.40 μg(r=0.999 8, n=6), and the regression equation was Y=114 166.67X+462 893.57, the average recovery was (99.51±0.67)% with a RSD of 0.67%. Conclusion: The method is simple, accurate and repeatable, and it can be used in the quality control of Xiaoyan Tablets. [Key words] HPLC; Xiaoyan Tablets; Baicalin; Content determination 消炎片主要由蒲公英、紫花地丁、野菊花、黄芩四味中药组成,具有抗菌消炎、清热解毒的作用,用于治疗呼吸道感染、发热、肺炎、支气管炎、咳嗽有痰、疖肿等。现质量标准收载于卫生部药品标准《中药成方制剂》第四册[1],标准中仅有定性鉴别,无处方药味特征成分的含量测定项目。本文通过参考有关资料,建立了高效液相色谱法测定黄芩中黄芩苷含量的方法,获得了很好的分离效果,本方法简单、准确、灵敏度高、重现性好,能够较原标准更好地控制药品质量。 1 仪器与试药 1.1 仪器 高效液相色谱仪(美国SP-8810,SP-100检测器,N2010色谱工作站)。 1.2 试药 消炎片(广西千珍制药有限公司,批号为080526、080714、081025);黄芩苷对照品(中国药品生物制品检定所,含量测定用,批号为110715-200514);乙腈为色谱纯,水为重蒸馏水,磷酸为分析纯。 2 方法与结果 2.1 色谱条件与系统适应性试验 色谱柱为Diamonsil C18柱(200 mm×4.6 mm,5 μm);流动相为乙腈-水-磷酸(32∶68∶0.2);检测波长为280 nm;流速为1.0 ml/min;柱温为室温;进样量为20 μl。灵敏度为0.1 AUFS,理论板数不低于3 000,此色谱条件下,峰形良好。 2.2 溶液的制备 2.2.1 对照品溶液的制备精密称取105℃恒温干燥3 h的黄芩苷对照品10 mg,置于50 ml容量瓶中,用甲醇溶解并稀释至刻度,摇匀,制成对照品储备液。精取2.0 ml,置10 ml容量瓶中,用甲醇溶解并稀释至刻度,摇匀,作为对照