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木贼的质量标准提升研究
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| 篇名： | 木贼的质量标准提升研究 |
| TITLE： | Study on Improvement of Quality Standard of Equisetum hyemale |
| 摘要： | 目的：为完善木贼药材的质量标准提供参考。方法：以来自不同产地的10批木贼药材为样品，采用薄层色谱（TLC）法对样品中的山柰酚-3-O-β-D-槐糖苷进行定性鉴别；参照2015年版《中国药典》附录的相关方法，测定样品中重金属、黄曲霉毒素、杂质、水分、总灰分、酸不溶性灰分、水溶性浸出物和醇溶性浸出物的含量；采用高效液相色谱（HPLC）法测定样品中山柰酚-3-O-β-D-槐糖苷含量，并建立木贼水溶性成分的HPLC指纹图谱。结果：TLC鉴别结果显示，在供试品色谱中，与山柰酚-3-O-β-D-槐糖苷对照品色谱相应位置上显相同颜色的荧光斑点，且空白对照无干扰。10批样品中杂质含量为0.19％～2.32％，水分含量为10.12％～11.87％，总灰分含量为6.67％～10.11％，酸不溶性灰分含量为1.34％～2.12％，水溶性浸出物含量为9.17％～13.99％，醇溶性浸出物含量为7.49％～13.68％；初步拟定杂质含量不得超过3.00％、总灰分含量不得超过10.00％、酸不溶性灰分含量不得超过2.50％、水溶性浸出物含量不得少于9.00％、醇溶性浸出物含量不得少于5.00％的标准。9批样品中检测出了砷（含量为0.064～0.225mg/kg），6批样品中检测出了镉（含量为0.106～0.132mg/kg），所有样品中均检测出了铅（含量为0.221～1.896mg/kg），但所有样品中均未检测到汞和黄曲霉毒素。HPLC方法学考察结果均符合《中国药典》相关要求；10批样品中山柰酚-3-O-β-D-槐糖苷含量为627.12～5384.53mg/kg，10批样品的HPLC指纹图谱相似度均大于0.900。结论：本研究新建了木贼中山柰酚-3-O-β-D-槐糖苷的定性、定量分析方法；对木贼中重金属、黄曲霉毒素、杂质等项目进行了检测，并对杂质、灰分和浸出物进行了限度拟定。所建方法简便、准确、重复性好，可用于木贼的质量控制。 |
| ABSTRACT： | OBJECTIVE：To provide reference for improving the quality sta ndard of Equisetum hyemale . METHODS ：Totally 10 batches of E. hyemale from different sites were collected as samples. TLC method was used to qualitatively identify kaempferol- 3-O-β-sophoroside. The contents of heavy metal ，aflatoxin，impurity，moisture，total ash ，acid-insoluble ash ，water-soluble extract and ethanol-soluble extract were determined according to supplementary provisions of Chinese Pharmacopoeia （2015 edition）. HPLC method was used to determine the content of kaempferol- 3-O-β-sophoroside in sample. HPLC fingerprint of water-soluble extract from E. hyemale was also established. RESULTS ：TLC identification showed that in the chromatogram of the test sample ， fluorescent spots with the same color were displayed on the corresponding positions of the chromatogram of substance control of kaempferol-3-O-β-sophoroside，and without interference from blank control. Among 10 batches of samples ，the contents of impurities were 0.19％-2.32％；the water contents were 10.12％-11.87％；the total ash contents were 6.67％-10.11％；the acid-insoluble ash contents were 1.34％-2.12％；the water-soluble extract contents were 9.17％-13.99％；the ethanol-soluble extract contents were 7.49％-13.68％，respectively. It is preliminarily proposed that the impurity content shall not exceed 3.00％；the total ash content shall not exceed 10.00％；the acid-insoluble ash content shall not exceed 2.50％；the water-soluble extract content shall not be less than 9.00％ ；the ethanol-soluble extract content shall not be less than 5.00％. Arsenic（0.064-0.225 mg/kg） 010815） was detected in 9 batches of samples ；cadmium（0.106-0.132 E-mail：cruise0303@163.com mg/kg）was detected in 6 batches of samples ；lead（0.221- 1.896 mg/kg）was detected in all samples ，but no mercury or rebecca aflatoxin was detected. The results of HPLC method met the relevant requirements of Chinese Pharmacopoeia . The content of kaempferol- 3-O-β-D-sophoroside in 10 batches of samples was 627.12-5 384.53 mg/kg，and the similarity of HPLC fingerprints of 10 batches of samples was more than 0.900. CONCLUSIONS ： A new qualitative and quantitative analysis method for kaempferol- 3-O-β-D-sophoroside was established ；the heavy metals ， aflatoxins，impurities and other items in E. hyemale were detected ；the limits of impurity ，ash and extract were determined. The established method is simple ，accurate and reproducible ，and can be used for quality control of E. hyemale . |
| 期刊： | 2020年第31卷第09期 |
| 作者： | 赖正权，艾伟鹏，胡震，窦耀星，蔡雨峰，刘伟，吴莹，张慈婷，谢晓琳，廖慧君 |
| AUTHORS： | LAI Zhengquan，AI Weipeng， HU Zhen，DOU Yaoxing，CAI Yufeng，LIU Wei，WU Ying，ZHANG Citing，XIE Xiaolin，LIAO Huijun |
| 关键字： | 木贼；山柰酚-3-O-β-D-槐糖苷；薄层色谱法；高效液相色谱法；指纹图谱；质量标准 |
| KEYWORDS： | Equisetum hyemale ；Kaempferol-3-O-β-sophoroside；TLC；HPLC；Fingerprint；Quality standard |
| 阅读数： | 315 次 |
| 本月下载数： | 9 次 |
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