奇应内消巴布剂定性定量方法研究

目的: 建立奇应内消巴布剂定性定量方法。 方法: 采用TLC法鉴别方中重楼、大黄、山柰;采用HPLC法测定大黄酸、大黄素、大黄酚含量。HPLC色谱条件:采用Agilent ZORBAX SB-C₁₈(4.6 mm×250 mm,5 μm)色谱柱,流动相为甲醇-0.2%磷酸水溶液(87∶ 13),流速1.0 mL·min^-1,检测波长440 nm,柱温30 ℃。 结果: 定性鉴别薄层色谱特征明显;HPLC测定,大黄酸浓度在4.00～25.00 μg·mL^-1范围内线性关系良好(r=0.9994),平均回收率(n=5)为98.39%(RSD=2.0%);大黄素浓度在17.92～112.00 μg·mL^-1范围内线性关系良好(r=0.9998),平均回收率(n=5)为97.25%(RSD=1.5%);大黄酚浓度在33.92～212.00 μg·mL^-1范围内线性关系良好(r=0.9992),平均回收率(n=5)为96.55%(RSD=1.8%)。 结论: 该法可以准确地对奇应内消巴布剂进行定性、定量检测,有效地控制该制剂的质量。

Objective: To establish the quality and quantity methods of Qiyingneixiao cataplasm. Methods: Parids Rhizoma,Rhei Radix et Rhizoma,Kaempferiae Rhizoma in this preparation were identified by TLC. The content of rhein,emodin and chrysophanol in Qiyingneixiao cataplasm were determined by HPLC. HPLC method was performed on a Agilent Zorbax SB C₁₈ column(4.6 mm×250 mm,5 μm) with a mobile phase of methanol-0.2% phosphoric acid. The wavelength of detector was set at 440 nm and the column temperature was 30 ℃. Results: Characteristics of identification were very obviously. The linear range of rhein was from 4.00 to 25.00 μg·mL^-1(r=0.9994) and the average recovery(n=5)was 98.39%(RSD=2.0%);The linear range of emodin was from 17.92 to 112.00 μg·mL^-1(r=0.9998) and the average recovery(n=5)was 97.25%(RSD=1.5%);The linear range of chrysophanol was from 33.92 to 212.00 μg·mL^-1(r=0.9992) and the average recovery(n=5)was 96.55%(RSD=1.8%). Conclusion: The methods of qualitative and quantitative analysis are accurate and suitable for effectively controlling quality of Qiyingneixiao cataplasm.

[1] ZHANG Hong-xia(张红霞),JIN Yi(金艺),XU Hai-yan(许海燕),et al.Determination of rhein,emodin,chrysophanol and rheochrysidin in Weili tablet by HPLC(HPLC法测定胃力片中大黄酸、大黄素、大黄酚和大黄素甲醚的含量).J Shenyang Pharm Univ(沈阳药科大学学报),2007,24(7):417
[2] WANG Xia(汪霞).RP-HPLC determination of rehin,emodin and chrysophanol in Huanglian Shangqing tablets(反相HPLC法测定黄连上清片中大黄酸、大黄素、大黄酚的含量).Chin J Pharm Anal(药物分析杂志),2008,28(8):1310
[3] CAO Hong(曹红),LIU Yun(刘云).Determination of rhein,emodin,chrysophanol,physcion and aloe-emodin in Jinyiniaoshi granules and Radix Rhei by HPLC(高效液相色谱法测定金薏尿石颗粒剂及大黄药材中大黄酸、大黄素、大黄酚、大黄素甲醚和芦荟大黄素的含量).Chin J Pharm Anal(药物分析杂志),1998,18(1):3
[4] XU Qian-li(许乾丽),MAO Xiang-jun(茅向军),SONG Xiao-ning(宋晓宁),et al.HPLC simultaneous determination of aloe-emodin,rhein,emodin,chrysophanol and physcion in Liuwei Anxiao capsules(HPLC法同时测定六味安消胶囊中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量).Chin J Pharm Anal(药物分析杂志),2010,30(10):1841
[5] ChP(中国药典).2010.Vol Ⅰ(一部):22,243