Page 87 - 2019年10月第30卷第20期

哈萨克药骆驼蓬草的质量标准研究 Δ

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许 欢 ，江阿古丽·艾山 ，汪 晶 ，李筱婧 ，陈 斌 ，木拉提·克扎衣别克 ，黄一平 （1.南京中医药大
3 #a
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学第三临床医学院，南京 210046；2.江苏省中医药研究院/国家中医药管理局中药释药系统重点研究室，南京
210028；3.伊犁哈萨克自治州中医医院/伊犁哈萨克自治州哈萨克医药研究所，新疆 伊宁 835000）
中图分类号 R282；R917 文献标志码 A 文章编号 1001-0408（2019）20-2818-06
DOI 10.6039/j.issn.1001-0408.2019.20.16
摘 要 目的：建立哈萨克药骆驼蓬草药材的质量标准。方法：以新疆哈萨克地区采集的10批骆驼蓬草药材为研究对象，考察其
性状；采用薄层色谱（TLC）法对药材中骆驼蓬碱和去氢骆驼蓬碱进行定性鉴别；采用2015版《中国药典》（四部）相关方法检查其
水分、总灰分、酸不溶性灰分和醇浸出物含量；采用高效液相色谱（HPLC）法测定药材中骆驼蓬碱和去氢骆驼蓬碱的含量，色谱柱
为X-bridge C18 （250 mm×4.6 mm，5 μm），流动相为乙腈-醋酸铵缓冲液（冰醋酸调节pH至6），梯度洗脱，检测波长为267 nm，柱温
为25 ℃，流速为1 mL/min，进样量为5 μL。结果：TLC法鉴别结果显示，10批药材在骆驼蓬碱和去氢骆驼蓬碱对照品相同位置处
均显示清晰斑点；水分、总灰分、酸不溶性灰分分别不得高于12％、22％、2％，醇浸出物不得低于16％。HPLC法考察结果显示，骆
驼蓬碱、去氢骆驼蓬碱分别在15.22～301.40、15.09～301.80 μg/mL质量浓度范围内线性关系良好，精密度、重复性、稳定性试验的
RSD均小于4％，平均回收率分别为100.22％、100.94％（RSD均小于2％）；含量测定结果显示，该药材总生物碱含量（以骆驼蓬碱、
去氢骆驼蓬碱合计）不得少于6.5 mg/g。结论：本研究在原标准基础上增加了检查项，建立了TLC法鉴别骆驼蓬碱、去氢骆驼蓬和
HPLC法测定两者含量的方法。所建质量标准可用于全面控制新疆哈萨克地区骆驼蓬草药材的质量。
关键词 骆驼蓬草；质量标准；检查；鉴别；骆驼蓬碱；去氢骆驼蓬碱；含量测定；薄层色谱法；高效液相色谱法

Study on Quality Standard for Kazakhstan Medicine Peganum harmala
XU Huan ，Jangagul·Asen ，WANG Jing ，LI Xiaojing ，CHEN Bin ，Murat·Kizaibek ，HUANG Yiping （1.
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School of Third Clinical Medicine，Nanjing University of TCM，Nanjing 210046，China；2. Jiangsu Province
Academy of TCM & Key Laboratory for TCM Drug Release System under State Administration of Traditional
Chinese Medicine，Nanjing 210028，China；3. TCM Hospital of Ili Kazakh Autonomous Prefecture & Kazakhstan
Medicine Institute of Ili Kazakh Autonomous Prefecture，Xinjiang Yining 835000，China）
ABSTRACT OBJECTIVE：To establish the quality standard for Kazakhstan medicine Peganum harmala. METHODS：Ten
batches of P. harmala collected in Xinjiang Kazakh region were selected as research objects to investigate their characteristics.
Qualitative identification of harmaline and harmine was conducted by TLC. The contents of water，total ash，acid-insoluble ash and
ethanol extract were tested according to Chinese Pharmacopoeia（2015 edition）. The contents of harmaline and harmine were
determined by HPLC. The determination was performed on X-bridge C18 column（250 mm × 4.6 mm，5 μ m）with mobile phase
consisted of acetonitrile-ammonium acetate buffer（adjusted to 6 with glacial acetic acid，gradient elution）at the flow rate of 1
mL/min. The detection wavelength was set at 267 nm，and column temperature was 25 ℃. The sample size was 5 μL. RESULTS：
TLC identification results showed that 10 batches of medicinal material showed clear spots at the same position as harmaline and
harmine reference substances. Water，total ash，acid-insoluble ash should not be more than 12％，22％，2％，respectively；ethanol
extract must not be less than 16％ . HPLC results showed that the linear ranges of harmaline and harmine were 15.22-301.40，
15.09-301.80 μg/mL；RSDs of precision，reproducibility and stability tests were all lower than 4％；average recoveries were 100.22％
and 100.94％（all RSD＜2％）. The determination results showed that the content of total alkaloids（harmaline and harmine）should
not be less than 6.5 mg/g. CONCLUSIONS：Based on the original standard，test items are added in this study. TLC method is
established to identify harmaline and harmine. HPLC method is established to determine their contents. Established quality standard
can be used for comprehensive quality control of P. harmala
Δ 基金项目：国家自然科学基金资助项目（No.81803756）；江苏省
研究生科研与实践创新计划（No.SJCX-0379） from Xinjiang Kazakh region.
＊硕士研究生。研究方向：中药药剂。E-mail：1678512159@qq. KEYWORDS Peganum harmala；Quality standard；Examina-
com tion；Identification；Harmaline；Harmine；Content determina-
#a 通信作者：研究员。研究方向：中药研究与开发。电话：025- tion；TLC；HPLC
85637809。E-mail：yipingh@163.com
#b 通信作者：研究员，博士。研究方向：哈萨克药资源调查与新
药研发。E-mail：murat_kizaibek@sina.com

·2818 · China Pharmacy 2019 Vol. 30 No. 20 中国药房 2019年第30卷第20期