清肺抑火片质量标准研究

Study on the Quality Standard of Qingfei Yihuo Tablet

目的:修订提高清肺抑火片的质量标准。方法:采用显微鉴别法、薄层色谱(TLC)法对制剂中的大黄、桔梗、黄柏、苦参进行定性鉴别;采用HPLC法对黄芩中的黄芩苷进行定量分析,色谱柱:Agilent TC-C18(250 mm×4.6 mm,5 m);流动相:甲醇-0.4%磷酸溶液(53:47);流速:0.6 m L/min;检测波长:280 nm;柱温:30℃。结果:在显微鉴别中检出草酸钙簇晶大,直径60~140μm(大黄)、菊糖扇形或类圆形(桔梗);在TLC色谱中检出大黄、黄柏、苦参;黄芩苷进样量在0.025~4.000μg/m L范围内线性关系良好,r=0.999 8;平均加样回收率99.8%,RSD=0.34%(n=9)。结论:所建立的方法可靠、准确、专属性强,可控制该制剂的质量。

Objective: To develop a method for revising and improving the quality standards of the Qingfei Yihuo Tablet. Methods:Microscopic identification and TLC method were adopted to identify the quality of the Dahuang, Jugeng, Huangbo and Kusheng in preparation and analyzing the Huangqigan in Huangqi by the method of HPLC. The analysis was performed on an Agilent TC-C18 column with the mobile phase consisting of methanol(A)?0.4% phosphate acid(53:47)by gradient elution at a flow rate of 0.6 mL/min. The detection wavelength was set at 280 nm and the column temperature was 30 ℃. Results: Calcium oxalate crystal clusters were checked out by the method of microscopic identification, the diameter of Dahuang was 60-140 microns and the shape of Jugeng was inulin fan or quasi-circular. Additional, Dahuang, Huangbo and Kusheng were detected out by the methods of TLC and the HPLC results showed that the linear ranges were 0.025-4.000 μg/mL(r=0.999 8)for Huangqigan. The average recoveries(n=9)were 99.8%, RSD=0.34%. Conclusion: The developed method is accurate, reproducible and specific and the quality of the preparation can be controlled.