正交试验法优选"支炎一号"合剂的制备工艺及质量标准研究
Optimization of the Preparation Process Using Orthogonal Experimental Design and Quality Standard Study of"Zhiyan No.1"Mixture
汤韦奇 1叶琛琛 1李文撼 1万国强 1裴昶1
作者信息
- 1. 宜兴市中医医院药学部,江苏 无锡 214200
- 折叠
摘要
目的 优选"支炎一号"合剂的制备工艺,对合剂中的中药材进行薄层色谱鉴别研究,同时建立橙皮苷的含量测定方法,并据此确定制剂的质量控制标准.方法 采用L9(34)正交试验法优选"支炎一号"合剂的水提取工艺,选取了加水量、浸泡时间、煎煮时间3个考察因素,以橙皮苷转移率和干膏率作为综合评价指标.并对合剂中的陈皮、射干、钩藤进行薄层色谱鉴别.采用高效液相色谱法,色谱柱选用Agilent ZORBAX SB C18,流动相为乙腈-水(21:79),流速:1 ml/min,柱温:40℃,检测波长:283 nm,测定橙皮苷的含量.结果 优选的最佳提取工艺为加水煎煮两次,分别加10倍和8倍量水,每次煎煮1 h.陈皮、射干、钩藤的薄层色谱鉴别分离度、重现性好、专属性强.橙皮苷进样量在0.050 41～0.756 21 µg范围内线性关系良好,回归方程为Y=2 145 448.558 6X-621.500 0,r2=0.999 8(n=6);稳定性、精密度良好,平均加样回收率为98.86％,相对标准偏差(RSD)为 1.2％(n=6).结论 此研究优选的制备工艺科学、合理,薄层色谱鉴别方法分离度好、专属性强,橙皮苷的含量测定方法准确可靠,适用于"支炎一号"合剂的制备及质量控制,为下一步的生产和合理用药提供可靠依据.
Abstract
Objective To optimize the preparation process of"Zhiyan No.1"mixture,conduct thin layer chromatography(TLC)identification research on the traditional Chinese medicinal materials in the mixture,establish a content determination method for hesperidin,and accordingly determine the quality control standards for the preparation.Methods The L9(34)orthogonal test method was used to optimize the water extraction process of"Zhiyan No.1"mixture.Three factors were considered:water addition,soaking time,and decoction time.The transfer rate of hesperidin and the dry extract rate were used as comprehensive evaluation indicators.TLC identification was performed on the traditional Chinese medicinal materials of tangerine peel,Belamcanda chinensis,and Uncaria rhynchophylla in the mixture.The high performance liquid chromatography(HPLC)method was employed,utilizing an Agilent ZORBAX SB C18 column.The mobile phase consisted of acetonitrile-water(21:79),with a flow rate of 1 ml/min,the column temperature was set at 40℃,and the detection wavelength was 283 nm,for the quantitation of hesperidin.Results The optimal extraction process was to add water and decoct twice,add 10 parts water and 8 parts water respectively,and cook for 1 hour each time.The TLC identification of tangerine peel,Belamcanda chinensis,and Uncaria rhynchophylla had good resolution,reproducibility,and strong specificity.Hesperidin has a good linear relationship within the sample injection range of 0.050 41～0.756 21 µg grams,and the regression equation was Y=2 145 448.558 6 X-621.500 0,r2=0.999 8(n=6).The stability and precision were good,and the average sample recovery rate of this product was 98.86％,with an RSD of 1.2％(n=6).Conclusion The optimized preparation process in this study is scientific and reasonable,and the thin layer chromatography identification has good resolution and strong specificity,quantitative determination method for hesperidin is accurate and reliable,which is suitable for the preparation and quality control of"Zhiyan NO.1"mixture and provides a reliable basis for the next step of production and rational drug use.
关键词
"支炎一号"/正交试验/制备工艺/薄层色谱/橙皮苷Key words
Zhiyan NO.1/Orthogonal test/Preparation technology/TLC/Hesperidin引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
万方数据