健脾消积颗粒提取工艺及质量标准研究

Extraction Technology and Quality Standards of Jianpi Xiaoji Granules

目的:优化健脾消积颗粒的提取工艺,建立其质量标准。方法:以柚皮苷和新橙皮苷的含量为主要评价指标,利用单因素考察和正交试验确定健脾消积颗粒的最佳提取工艺。将枳壳和莪术作为指标成分建立样品的薄层色谱法(TLC);测定样品的水分、粒度和溶化性;使用高效液相色谱法(HPLC)同时测定该样品中柚皮苷和新橙皮苷的含量。结果:健脾消积颗粒的最佳提取工艺为10倍量水煎煮2次,第1次2 h、第2次1 h,稠膏相对密度为1.20~1.25(70℃);枳壳和莪术的TLC图斑点清晰且阴性样品无干扰;6批样品的水分为2.80%~3.78%,粒度为1.29%~4.97%,溶化性为全部溶化,无异物、无焦屑;HPLC测定柚皮苷、新橙皮苷质量浓度分别为9.78~97.80、10.34~103.40μg·mL^(-1)时与峰面积线性良好,加样回收率分别为99.31%~100.69%(RSD=0.49%)、99.69%~100.98%(RSD=0.47%),精密度、稳定性、重复性的RSD均小于2%,每袋健脾消积颗粒样品中柚皮苷不得少于20 mg、新橙皮苷不得少于12 mg。结论:该方法重复性好、专属性强,可用于控制健脾消积颗粒的质量。

Objective:To optimize the extraction process of Jianpi Xiaoji Granules and establish quality standards for Jianpi Xiaoji Granules.Methods:With the content of naringin and neohesperidin as the main evaluation indicators,the optimal extraction process was determined by single-factor investigation method and orthogonal experiment.Aurantii Fructus and Curcumae Rhizoma were used as index components to establish a thin-layer chromatography(TLC)identification method for samples.The moisture,particle size,and solubility of the sample were determined.High-performance liquid chromatography(HPLC)was used to determine the content of naringin and neohesperidin in the sample simultaneously.Results:The optimal extraction process of Jianpi Xiaoji Granules involved decocting with 10 times the amount of water twice,for 2 hours the first time and 1 hour the second time,with a relative density of the dense paste of 1.20-1.25 at 70℃.The TLC spots of Aurantii Fructus and Curcumae Rhizoma were clear and had no interference in the negative controls,which can be used as a thin-layer identification of Jianpi Xiaoji Granules.The moisture content of six batches of samples was 2.80%-3.78%,the particle size was 1.29%-4.97%,and the solubility showed complete dissolution,with no foreign matter or scorched residue.HPLC results indicated that naringin showed good linearity in the range of 9.78-97.80μg·mL^(-1) and neohesperidin in the range of 10.34-103.40μg·mL^(-1),and the sample recovery rates were 99.31%-100.69%(RSD=0.49%)and 99.69%-100.98%(RSD=0.47%),respectively.The RSDs of precision,stability,and repeatability were less than 2%.The naringin in each bag of samples shall not be less than 20 mg,and the neohesperidin shall not be less than 12 mg.Conclusion:This method has good repeatability and exclusivity and can be used to control the production quality of Jianpi Xiaoji Granules.