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地龙药材的质量标准提升研究 Δ
王莎莎 ,曲 悦 ,薛大权 ,李兰清 ,向 阳 ,张宝徽 (1.湖北中医药大学药学院,武汉 430065;2.健民药业
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集团股份有限公司,武汉 430050)
中图分类号 R282 文献标志码 A 文章编号 1001-0408(2019)17-2379-05
DOI 10.6039/j.issn.1001-0408.2019.17.15
摘 要 目的:为完善和提高地龙药材的质量标准提供参考。方法:采用高效液相色谱(HPLC)法测定药材样品中次黄嘌呤、肌苷
的含量,同时按“中药色谱指纹图谱相似度评价系统”(2012版)软件建立地龙药材的HPLC指纹图谱并进行相似度评价。色谱柱
为Purospher STAR RP-18 endcapped;流动相为甲醇-水(梯度洗脱);流速为1 mL/min;检测波长为248 nm;柱温为30 ℃;进样量为
20 μL。结果:含量测定方法学考察结果显示,次黄嘌呤、肌苷的检测质量浓度线性范围分别为 1.58~31.6 μg/mL(r=0.999 9)、
5.52~110.4 μg/mL(r=0.999 8);定量限分别为0.316、0.552 μg/mL;检测限分别为0.158、0.110 μg/mL;精密度、稳定性(24 h)、重复
性试验的RSD均小于2.0%(n=6);平均回收率分别为103.0%(RSD=1.7%,n=6)、101.2%(RSD=1.2%,n=6)。成功建立了15
批样品的HPLC指纹图谱,共确定了8个共有色谱峰。其中有14批样品的HPLC指纹图谱与对照图谱R的相似度>0.900。结论:
建立的次黄嘌呤、肌苷含量测定及地龙药材HPLC指纹图谱方法简便、准确、重复性好,可用于地龙药材的质量控制。
关键词 地龙;次黄嘌呤;肌苷;高效液相色谱法;指纹图谱;质量标准
Study on Quality Standard Improvement of Pheretima
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WANG Shasha ,QU Yue ,XUE Daquan ,LI Lanqing ,XIANG Yang ,ZHANG Baohui(1.School of Pharmacy,
Hubei University of TCM,Wuhan 430065,China;2.Jianmin Pharmaceutical Group Co.,Ltd.,Wuhan 430050,
China)
ABSTRACT OBJECTIVE:To provide reference for improving the quality standard of Pheretima. METHODS:The contents of
hypoxanthine and inosine in medicinal material samples were determined by HPLC. HPLC fingerprint of Pheretima was established
according to “Similarity evaluation system for TCM chromatogramtic fingerprint”(2012 edition) software, and similarity
evaluation was conducted. The determination was performed on Purospher STAR RP-18 endcapped with mobile phase consisted of
methanol-water (gradient elution) at the flow rate of 1 mL/min. The detection wavelength was 248 nm,and the column
temperature was set at 30 ℃ . The sample size was 20 μ L. RESULTS:The results of methodological investigation of content
determination showed that the linear range of hypoxanthine and inosine were 1.58-31.6 μg/mL(r=0.999 9),5.52-110.4 μg/mL(r=
0.999 8),respectively. limits of quantify were 0.316,0.552 μg/mL,respectively;limits of detection were 0.158,0.110 μg/mL,
respectively;RSDs of precision,stability(24 h)and repeatability tests were all less than 2.0%(n=6). Average recovery rates
were 103.0%(RSD=1.7%,n=6)and 101.2%(RSD=1.2%,n=6),respectively. HPLC fingerprint for 15 batches of samples
were established,and 8 common peaks were identified. The similarity of HPLC fingerprint of 14 batches of sample with control
fingerprint R was higher than 0.900. CONCLUSIONS:The established method for content determination of hypoxanthine and
inosine and HPLC fingerprint of Pheretima are simple,accurate and reproducible,and can be used for quality control of Pheretima.
KEYWORDS Pheretima;Hypoxanthine;Inosine;HPLC;Fingerprint;Quality standard
[2]
地龙为钜蚓科动物参环毛蚓[Pheretima aspergillum 于《神农本草经》 ,称“白颈蚯蚓”,被列为下品。而地龙
[3]
(E. Perrier)]、通俗环毛蚓(Pheretima vulgaris Chen)、威 的名称始记载于《图经本草》 ,曰:“白颈蚯蚓生平土,今
廉环毛蚓[Pheretima guillelmi(Michaelsen)]或栉盲环毛 处处平泽膏壤土中皆有之,……方家谓之地龙”。现代
蚓(Pheretima pectinifera Michaelsen)的干燥体。前一种 药理学研究表明,地龙具有溶栓、抗凝血、抗心律失常、
习称“广地龙”,后3种习称“沪地龙”,其性寒,味咸,具有 降压、镇静、抗惊厥、解热、镇痛、抗炎、抗肿瘤和止咳平
清热定惊、通经活络、平喘利尿的功效 。地龙药用始载 喘等多种药理作用 [4-7] 。研究表明,核苷类成分是地龙舒
[1]
Δ 基金项目:国家中医药管理局中药重点产品行业标准制定计划 张支气管、抗组胺、平喘的重要药用物质基础,也对人体
(No.ZYY-2017-018) 的代谢和免疫有着重要作用 [8-9] ,其中次黄嘌呤的含量与
*硕士研究生。研究方向:药物新制剂、新剂型及新技术。E- [5]
地龙药材止咳化痰、平喘的药效作用成正相关 ,而肌苷
mail:wangshasha123wh@163.com
有免疫调节和神经保护作用 [10-11] 。
# 通信作者:副教授,硕士生导师,博士。研究方向:中药及其制
剂的物质基础。E-mail:24662873@qq.com 2015年版《中国药典》(一部)中地龙项下有性状、鉴
中国药房 2019年第30卷第17期 China Pharmacy 2019 Vol. 30 No. 17 ·2379 ·