摘要
目的:建立鹿药的质量标准。方法:从原植物形态、性状特征、显微特征、薄层色谱(TLC)等方面对药材进行定性鉴别;测定药材的水分、灰分、浸出物;采用高效液相色谱法测定药材中(25S)-17α-羟基-5α-螺甾烷-9-烯-3β-O-β-D-葡萄吡喃糖基-(1→2)-[β-D-木吡喃糖基(1→3)]-β-D-葡萄吡喃糖基(1→4)-β-D-半乳吡喃糖苷(SJ-13)的含量,色谱柱为Waters SunFire C18,流动相为乙腈-水(35∶65,V/V),流速为1.0 mL/min,检测波长为203 nm,柱温为20℃,进样量为10μL。结果:原植物为多年生草本植物,高30～60 cm;药材表面呈棕色至棕褐色,具皱纹;显微特征为表皮1列细胞;药材粉末呈灰黄色,含大量草酸钙针晶。药材样品的TLC图斑点大部分清晰,分离度好;药材中水分为5.26%～8.88%,总灰分为4.60%～28.86%,酸不溶性灰分为1.56%～23.39%,水浸出物为23.84%～51.26%,醇浸出物为22.65%～57.36%;SJ-13检测进样量线性范围为8.92～31.22μg(r=0.999 9),精密度、稳定性、重复性试验的RSD均小于1%,加样回收率为97.0%～99.2%(RSD=0.8%,n=6),耐用性试验的RSD均小于1%,10批药材样品中SJ-13的含量范围为4.40～29.80 mg/g。结论:初步拟定鹿药药材中水分不得过11%,总灰分不得过35%,酸不溶性灰分不得过28%,水浸出物不得少于19%,醇浸出物不得少于18%,SJ-13含量不得少于4.40 mg/g;该试验所建标准可用于鹿药的质量控制。
OBJECTIVE:To establish the quality standard of Smilacina japonica.METHODS:S.japonica was identified qualitatively in respects of original plant morphology,character,microscopic identification,TLC,etc.The moisture,ash and extract of medicinal materials were determined.The content of(25S)-17α-hydroxy-5α-spirostane-9-ene-3β-O-β-D-glucopyranoyl-(1→2)-[β-D-xylanosyl(1→3)]-β-D-glucopyranoyl(1→4)-β-D-galactopyranoside(SJ-13)was determined by HPLC.The determination was performed on Waters SunFire C18 column with mobile phase consisted of acetonitrile-water(35∶65,V/V)at the flow rate of 1.0 mL/min.The detection wavelength was set at 203 nm and the column temperature was 20℃.The sample size was 10μL.RESULTS:The original plant was perennial herbal,with height of 30-60 cm.The surface of the medicinal material was brown to brownish brown,with wrinkle and 1 row cells in epidermis.The powder of medicinal material was grayish yellow and contained large amount of acicular crystal.TLC spots were clear and well-separated.The content of moisture was 5.26%-8.88%;the content of total ash was 4.60%-28.86%;the acid-insoluble ash was 1.56%-23.39%,water extract was 23.84%-51.26%and alcohol extract was 22.65%-57.36%.The linear range of SJ-13 were 8.92-31.22μg(r=0.999 9).RSDs of precision,stability and reproducibility tests were all lower than 1%.The average recoveries were 97.0%-99.2%(RSD=0.8%,n=6).RSD of durability test was lower than 1%.The content of SJ-13 was 4.40-29.80 mg/g in 10 batches of medicinal samples.CONCLUSIONS:The content of water,total ash,acid insoluble components should not exceed 11%,35%,28%;the content of water extract,alcohol extract and SJ-13 should not be less than 19%,18%and 4.40 mg/g,respectively.Established standard can be used for the quality control of S.japonica.
作者
崔誉文
刘银环
热萨莱提·图尔孙
毛昭琦
宋小妹
CUI Yuwen;LIU Yinhuan;Resalaiti·TUERSUN;MAO Zhaoqi;SONG Xiaomei;CUI Yuwen(School of Pharmacy,Xi’an Medical University,Xi’an 710021,China;College of Pharmacy,Shaanxi University of TCM,Shaanxi Xianyang 712046,China)
出处
《中国药房》
CAS
北大核心
2018年第20期2786-2790,共5页
China Pharmacy
基金
陕西省教育厅重点实验室科研计划项目(No.17JS030)。
