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木贼的质量标准提升研究 Δ

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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 （1.深圳大学总医
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院药学部，广东 深圳 518055；2.香港中文大学中医学院，香港；3.广州中医药大学中医药数理工程研究院，广
州 510006；4.华中科技大学协和深圳医院/深圳大学第六附属医院药学部，广东 深圳 518052）
中图分类号 R282 文献标志码 A 文章编号 1001-0408（2020）09-1080-06
DOI 10.6039/j.issn.1001-0408.2020.09.11
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0.064～0.225 mg/kg），6批样品中检测出了镉（含量为0.106～0.132 mg/kg），所有样品中均检测出了铅（含量为0.221～
1.896 mg/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627.12～5 384.53 mg/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。
关键词 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

Study on Improvement of Quality Standard of Equisetum hyemale
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LAI Zhengquan ，AI Weipeng ，HU Zhen ，DOU Yaoxing ，CAI Yufeng ，LIU Wei ，WU Ying ，ZHANG Citing ，
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XIE Xiaolin ，LIAO Huijun（1.Dept. of Pharmacy，Shenzhen University General Hospital，Guangdong Shenzhen
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518055，China；2.School of Chinese Medicine，the Chinese University of Hong Kong，Hong Kong，China；3.
Mathematical Engineering Academy of Chinese Medicine，Guangzhou University of TCM，Guangzhou 510006，
China；4.Dept. of Pharmacy，Union Shenzhen Hospital，Huazhong University of Science and Technology/the
Sixth Affiliated Hospital of Shenzhen University，Guangdong Shenzhen 518052，China）
ABSTRACT OBJECTIVE：To provide reference for improving the quality standard 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
Δ 基金项目：广东省自然科学基金面上项目（No.2019A1515-
shall not be less than 5.00％ . Arsenic （0.064-0.225 mg/kg）
010815）；广东省教育科学“十三五”规划项目（No.2018KQNCX216）
was detected in 9 batches of samples；cadmium（0.106-0.132
＊主管中药师，助理研究员，博士。研究方向：中药抗肿瘤。
E-mail：cruise0303@163.com mg/kg） was detected in 6 batches of samples；lead （0.221-
# 通信作者：主管中药师，博士。研究方向：中药抗肿瘤。E-mail： 1.896 mg/kg）was detected in all samples，but no mercury or
rebecca200202@163.com aflatoxin was detected. The results of HPLC method met the

·1080 · China Pharmacy 2020 Vol. 31 No. 9 中国药房 2020年第31卷第9期