山楂冷冻干燥工艺及质量标准研究

为保护山楂有效成分及营养成分,采用真空冷冻干燥方式加工山楂饮片,并建立冻干山楂饮片中以枸橼酸为检测指标的高效液相色谱法.在单因素试验基础上,通过正交试验优化山楂冷冻干燥工艺;高效液相色谱法的流动相为磷酸二氢铵-磷酸缓冲液(pH为3.0),检测波长为210 nm,柱温为25℃,流速为1.0 mL/min,进样量为10μL.实验结果表明,冻干山楂最佳工艺为物料厚度75 mm,升温速率3.0℃/h,预冻时间6 h,解析温度60℃;枸橼酸在25~2 500μg/mL范围内线性关系良好,平均回收率为96.72%,RSD为1.19%.实验结果显示,优选的山楂真空冷冻干燥工艺稳定可行;建立的高效液相色谱法灵敏快捷,准确度高,可用于控制山楂冻干饮片的质量.

Study on Technology and Quality Standard of Freeze-Dried Hawthorn

In order to preserve the effective ingredients and the nutrition in hawthorn,vacuum freeze-drying is used to process the hawthorn tablets and to establish a high-performance liquid chromatography(HPLC)method by taking the citric acid as the indicator in freeze-dried hawthorn tablets.Based on the single factor test,the freeze-drying process was optimized by orthogonal test.The high performance liquid chromatography was used,and the mobile phase was sodium dihydrogen phosphate-phosphate buffer(pH 3.0),the detection wavelength was 210 nm,the column temperature was 25℃,the flow rate was 1.0 mL/min,and the sample amount was 10μL.The results showed that the best process for freeze-drying hawthorn was:when the thickness of the material was 75 mm,the speed of temperature increase was 3.0℃/h,pre-freezing time was 6 h and the analytical temperature was 60℃.The linear relationship was good in the range of 25-2500 ug/mL,the average recovery rate was 96.72%and the RSD was 1.19%.The experimentd results show that the optimal freeze-drying process is stable and feasible.The established HPLC method is sensitive and rapid with high accuracy.Therefore,it can be used to control the quality of freeze-dried hawthorn tablets.