广西产拳卷地钱水分灰分浸出物限量测定和薄层色谱研究
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摘要
目的:为了限制药材中含水量和泥沙等杂质及为了鉴别药材的真伪,更全面地控制广西产拳卷地钱质量,该实验对其水分、灰分和浸出物进行限量测定及薄层色谱鉴定方法进行研究。方法:按照2015年版《中华人民共和国药典》(第四部)0832项下水分测定法、2302项下灰分测定法、2201项下浸出物测定法和0502项下薄层色谱法,对广西产拳卷地钱进行水分灰分浸出物限量测定和考察其TLC条件,建立其薄层色谱鉴定方法。结果:广西不同产地10批拳卷地钱水分含量在4.86%～9.44%,总灰分含量在14.78%～19.99%范围内,酸不溶性灰分含量在1.77%～4.80%范围内,50%乙醇热浸出物的含量在12.11%～20.01%。薄层色谱鉴别结果显示:展开剂为氯仿∶甲醇(7∶0.5),以芹菜素为对照品,用5%三氯化铝乙醇显色再结合荧光灯(365 nm)下检视,广西不同产地10批药材与芹菜素对照品在相同的位置上分离出一个相同的黄色荧光斑点。结论:该方法简便、数据准确、重复性良好,为广西产拳卷地钱质量评价的研究奠定基础,也为今后拳卷地钱药材质量标准的建立提供了参考依据。
Objective:To control the quality of Guangxi fist volume more comprehensively in order to restrict the impurities such as water content and sediment in the medicinal materials and to identify the authenticity of the medicinal materials,this experiment has carried on the research on the determination of the water,ash and extract and the identification method of thin layer chromatography in this experiment. Methods:in accordance with the 2015 edition of the Chinese Pharmacopoeia(fourth parts),0832 items of water determination,2302 ash determination,2201 lower leaching substances and 0502 thin layer chromatography,the limit determination of water ash extracts of Guangxi fist volume and the inspection of its TLC pieces were carried out. Results:The water content of the 10 batches of fist rolls in Guangxi is from 4.86% to 9.44%,the total ash content is within the range of 14.78% to 19.99%,the acid insoluble ash content is within the range of 1.77% to 4.80%,and the content of the 50% ethanol thermal extract is 12.11% to 20.01%. The TLC identification results showed that the unfolding agent was chloroform:methanol(7∶0.5),with apigenin as the control,and 5% aluminum trichloride ethanol color re binding fluorescent lamp(365 nm). The same yellow fluorescent spots were separated from 10 batches of Guangxi origin and apigenin control in the same position. Conclusion:the method is simple,accurate and reproducible,which lays the foundation for the study of the quality evaluation of Guangxi fist volume,and also provides a reference for the establishment of the quality standard of Chinese medicinal materials in the future.
Objective:To control the quality of Guangxi fist volume more comprehensively in order to restrict the impurities such as water content and sediment in the medicinal materials and to identify the authenticity of the medicinal materials,this experiment has carried on the research on the determination of the water,ash and extract and the identification method of thin layer chromatography in this experiment. Methods:in accordance with the 2015 edition of the Chinese Pharmacopoeia(fourth parts),0832 items of water determination,2302 ash determination,2201 lower leaching substances and 0502 thin layer chromatography,the limit determination of water ash extracts of Guangxi fist volume and the inspection of its TLC pieces were carried out. Results:The water content of the 10 batches of fist rolls in Guangxi is from 4.86% to 9.44%,the total ash content is within the range of 14.78% to 19.99%,the acid insoluble ash content is within the range of 1.77% to 4.80%,and the content of the 50% ethanol thermal extract is 12.11% to 20.01%. The TLC identification results showed that the unfolding agent was chloroform:methanol(7∶0.5),with apigenin as the control,and 5% aluminum trichloride ethanol color re binding fluorescent lamp(365 nm). The same yellow fluorescent spots were separated from 10 batches of Guangxi origin and apigenin control in the same position. Conclusion:the method is simple,accurate and reproducible,which lays the foundation for the study of the quality evaluation of Guangxi fist volume,and also provides a reference for the establishment of the quality standard of Chinese medicinal materials in the future.
引文
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[14]周雨晴,杜沛霖,王跃峰,等.拳卷地钱基因组DNA提取及ISSR-PCR扩增体系优化[J].时珍国医国药,2014,25(6):1498-1500.
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[2]夏征农.辞海[M].上海:上海辞书出版社,1999:639.
[3]朱华.广西地钱属药用植物资源调查和形态构造研究[C]//第三届全国《中药鉴定学》研讨会论文集.成都:成都中医药大学,2002:161-165.
[4]朱华,邹登峰,黄海滨,等.拳卷地钱中芹菜素的测定[J].化工技术与开发,2005,21(2):30-32,43.
[5]朱华,肖建波,邹登峰,等.硅胶柱色谱/RP-HPLC/LC-ESI-MS分离纯化鉴定拳卷地钱中芹菜素-7-O-β-D-葡萄糖醛酸苷[J].中医药学刊,2005,12(1):20-22.
[6]王跃峰,杜沛霖,谢凤凤,等.广西产拳卷地钱资源调查研究[J].大众科技.2017,26(9):12-26.
[7]曹慧,蒋新宇,肖建波.拳卷地钱挥发油成分分析[J].广西植物,2005,25(6):596-597.
[8]朱华,邹登峰,肖建波,等.拳卷地钱总黄酮的提取与纯化[J].食品科学,2005,11(10):156-159.
[9]肖建波,朱华,钟世安,等.反相高效液相色谱法用于拳卷地钱中黄酮类化合物的分离和测定[J].分析试验室,2005,24(4):17-19.
[10]童星,陈晓青,蒋新宇,等.微波法和法多索法提取拳卷地钱中总黄酮的研究[J].中成药,2008,30(4):625-627.
[11]肖建波,曹慧,向海艳,等.拳卷地钱中黄酮类化合物的含量测定(英文)[J].天然产物研究与开发,2005,17(2):186-189,194.
[12]肖建波.拳卷地钱中脂溶性成分的分离纯化、结构表征及生物活性研究[D].长沙:中南大学,2005.
[13]王跃峰,张可锋,周雨晴,等.拳卷地钱总黄酮对四氯化碳致急性肝损伤大鼠的保护作用及其作用机制[J].时珍国医国药,2017,28(2):277-279.
[14]周雨晴,杜沛霖,王跃峰,等.拳卷地钱基因组DNA提取及ISSR-PCR扩增体系优化[J].时珍国医国药,2014,25(6):1498-1500.
[15]张海珠,周浓,李海峰.云连药材水分、灰分和浸出物的含量测定[J].大理学院学报,2011,30(12):38-40.
[16]国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:6.