鹿药的质量标准研究
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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(25 S)-17 α-hydroxy-5 α-spirostane-9-ene-3 β-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 10 μ L.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 8.92-31.22 μg(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.
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(25 S)-17 α-hydroxy-5 α-spirostane-9-ene-3 β-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 10 μ L.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 8.92-31.22 μg(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.
引文
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[11]平华. HPLC法同时测定生脉散中4种人参皂苷类成分的含量[J].中国药房,2016,27(12):1702-1704.
[12]LIU X,ZHANG H,NIU XF,et al. Steroidal saponin from Smilacina Japonica[J]. Fitoterapia,2012,83(4):812-816.
[13]国家药典委员会.中华人民共和国药典:四部[S]. 2015年版.北京:中国医药科技出版社,2015:57、103、202、204.
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[15]刘霞,岐琳,李延,等.大孔吸附树脂纯化鹿药总皂苷和总黄酮的研究[J].西北药学杂志,2012,27(6):516-519.
[2]李萍,任红莉.陕西地产“七药”[J].世界最新医学信息文摘,2003,3(2):682.
[3]葛宝福,张绪成,苏峰,等.集安市山野菜植物名录[J].中国园艺文摘,2011(9):56.
[4]宋小妹,刘海静.太白七药研究与应用[M].北京:人民卫生出版社,2011:239-244.
[5]吉海旺.“七”药在风湿类疾病治疗中的应用[C]//首届中国中西医结合风湿病西北学术会议暨培训班论文汇编,2011:41.
[6]赵淑杰,韩梅,韩忠明,等.高速逆流色谱分离与鉴定鹿药中黄酮类化合物[J].分析化学研究简报,2009,37(9):1345-1347.
[7]安晓云,慈嘉,申琼.鹿药组织培养的研究[J].中国园艺文摘,2010(10):14.
[8]赵淑杰,韩忠明,李彦颖,等.鹿药提取物清除羟基自由基的研究[J].华南农业大学学报,2010,31(2):59-62.
[9]赵淑杰,洪波,韩忠明,等.鹿药化学成分及其抗肿瘤活性[J].中成药,2016,38(2):332-335.
[10]宋小妹,刘海静.太白七药研究与应用[M].北京:人民卫生出版社,2011:269-273.
[11]平华. HPLC法同时测定生脉散中4种人参皂苷类成分的含量[J].中国药房,2016,27(12):1702-1704.
[12]LIU X,ZHANG H,NIU XF,et al. Steroidal saponin from Smilacina Japonica[J]. Fitoterapia,2012,83(4):812-816.
[13]国家药典委员会.中华人民共和国药典:四部[S]. 2015年版.北京:中国医药科技出版社,2015:57、103、202、204.
[14]赵淑杰,杨利民.鹿药中总黄酮含量的测定[J].安徽农业科学,2010,38(33):18756-18758.
[15]刘霞,岐琳,李延,等.大孔吸附树脂纯化鹿药总皂苷和总黄酮的研究[J].西北药学杂志,2012,27(6):516-519.