珍黄胃片质量标准提升的研究

Study on Improvement of Quality Standard of Zhenhuangwei Tablets

目的:建立珍黄胃片的制酸力检查方法和含量测定方法,对其质量标准进行完善提高。方法:采用回滴定的方法测定珍黄胃片的制酸力,控制温度为37℃,振摇速度为150 r/min,振摇时间为1 h,以溴酚蓝指示剂(黄→蓝紫)为指示滴定终点;采用高效液相色谱法,以大黄素和大黄酚为检测指标建立大黄的定量测定方法,色谱柱为phenomenex luna C18(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(82∶18),流速为1.0 mL/min,柱温为30℃,检测波长为439 nm,进样量为20μL。结果:测得12批珍黄胃片制酸力为30~36 mL/片,平均制酸力为33 mL/片;含量测定方法中大黄素的进样量在0.0406~0.812μg(r=1.0000)、大黄酚的进样量在0.0808~1.616μg(r=1.0000)的范围内均与各自的峰面积呈良好的线性关系;经低、中、高三个浓度的准确度试验考察,大黄素的回收率为95%~100%,大黄酚的回收率为95%~103%。结论:建立的制酸力检查方法和含量测定方法操作简单,具有良好的重复性和准确性,且专属性强,为该品种质量标准的提高奠定研究基础。

Objective To establish anacid-consuming capacity method and a content determination method for Zhenhuangwei Tablets,in order to improve the quality standard of Zhenhuangwei Tablets. Methods The acid-consuming capacity of Zhenhuangwei Tablets was determined by neutral titration. The experimental temperature was controlled at 37 ℃, the shaking speed was 150 r·min-1, the shaking time was 1 hour, and the bromophenol blue indicator(yellow→blue-violet) was used as the indicator end point. Emodin and Chrysophanol which were taken as index components in Rheum Off-icinale was determined by HPLC. The chromatographie column was phenomenex luna C18(2)(250 mm×4.6 mm, 5 μm), the mobile phase was methanol-0.1% phosphoric acid solution(82∶18),the flow rate was 1.0 mL·min-1,the column temperature was 30 ℃,the detection wavelength was set at 439 nm, and the injection amount was 20 μL. Results The acid-consuming capacity of 12 batches of Zhenhuangwei Tablets was measured to be 30 mL/table to 36 mL/tablet,and the average acid-consuming capacity was 33 mL/table. The linearrang of emodin was 0.0406-0.812 μg(r=1.0000), and the The linearrang of chrysophanol was 0.0808~ 1.616 μg(r=1.0000). At 3 concentration levels the recovery of emodinwas 95%~100% and the recovery of e chrysophanolwas 95%~103%. Conclusion The acid-consuming capacity method and content determination method are simple accurate, it have good repeatability and accuracy, and have strong specificityWhich can laya reaserrch foundation for the improvement of quality standard of Zhenhuangwei Tablets.