维药骆驼蓬草质量标准研究  

Research on quality standards of herbs of Peganum harmala

作　　者：温方方[1] 郑立明[2] 李晓静[3] 李岩[3] 张磊[1] 程雪梅[1] 王长虹[1] 王峥涛[1] 

机构地区：[1]海中医药大学中药研究所中药标准化教育部重点实验室中药新资源与质量标准综合评价国家中医药管理局重点研究室上海中药标准化研究中心,上海201203 [2]新疆医科大学第五附属医院,新疆乌鲁木齐830011 [3]新疆医科大学药学院药剂物化教研室,新疆乌鲁木齐830011

出　　处：《中国中药杂志》2012年第19期2971-2976,共6页China Journal of Chinese Materia Medica

基　　金：国家自然科学基金项目(81173119);国家自然科学基金-新疆联合基金重点项目(U1130303);国家“重大新药创制”科技重大专项(2012ZX09103201-051);国家药典委员会2010药典标准提高项目(507,508)

摘　　要：目的:建立维药骆驼蓬草的质量标准。方法:参照2010年版《中国药典》附录相关方法,对骆驼蓬草水分、总灰分、水溶性浸出物、酸不溶性灰分和重金属进行检测。采用硅胶HSGF254薄层板上,以乙酸乙酯-甲醇-氨水(10∶1.5∶0.5)为展开剂,分别采用置紫外光(254 nm)下检视、碘化铋钾显色以及乙酰胆碱脂酶导向的薄层色谱-生物自显影技术对骆驼蓬草进行鉴别。采用C18色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.1%三氟乙酸溶液(15∶85)为流动相,在280 nm波长下对骆驼蓬草中活性成分鸭嘴花碱进行定量分析。结果:采用紫外光(254 nm)下检视及乙酰胆碱脂酶生物自显影技术可对骆驼蓬草中的活性成分进行定性鉴别。鸭嘴花碱在0.7923～792.3 mg.L-1呈良好的线性关系,方法平均回收率为101.6%,RSD为1.9%,方法的日内和日间精密度均小于2%。10批骆驼蓬草中鸭嘴花碱质量分数在0.23%～1.47%,波动较大。结论:根据结果制定了药材中鸭嘴花碱的质量分数限度不得低于0.6%。水分、总灰分、酸不溶性灰分、水溶性浸出物分别不得过10.0%,20.0%,1.7%和30.0%。重金属铅、镉、砷、汞、铜分别不得过5,3,2,2,20 mg.kg-1。建立的定性和定量方法可用于维药骆驼蓬草药材的质量控制。Objective： To establish the quality standards of the herbs of Peganum harmala. Method： According to the Chinese Pharmacopoeia（2010 Version, Volume 1） and its appendix method, the water, total ash, acid insoluble ash, water-soluble extractives, and heavy metal were analyzed for herbs of P. harmala. TLC method was used to separate harmaline, harmine and vasicine from the herb samples by mixture of ethyl acetate-methanol-ammonia（10：1.5：0.5） as a developing solvent on high performance silica gel precoated plate（HSGF254） and to identify them inspected under UV 366 nm, visualized by spraying with both Dragendorff reagent, and by bioautographic assay. In the HPLC method, vasicine was separated on a C18（4.6 mm×250 mm, 5 μm） column with metnanol-0.1% trifluoroacetic acid（15：85） as the mobile phase and detected at at 280 nm. Result： In the TLC procedures, 254 nm fluorescent and bioautographic assay for the detection of acetylcholinesterase inhibitor can be used for the qualitative identification of the active ingredients. For the HPLC quantitation method, the calibration curve of vasicine displayed ideal linearity over the range of 0.792 3-792.3 mg·L-1 with the regression equation of Y=18 227X-24.879（r=0.999 9）. The average recovery of vasicine was 101.6% with a RSD of 1.9%. The RSD values of intra-day and inter-day precision were less than 2%. The content of vasicine in 10 batches of herbs of P. harmala fluctuates between 0.23% and 1.47%. Conclusion： The results indicated that the limit of vasicine was not lower than 0.6%,and the water, total ash, acid insoluble ash, and water-soluble extractives were not more than 10.0%, 20.0%, 1.7%, and 30.0%, respectively. The heavy metal of plumbum, cadmium, arsenic, mercury, and copper were not more than 5, 3, 2, 2, and 20 mg·kg-1, respectively. The qualitative and quantitative method established was suitable for the quality evaluation and assessment of herbs of P. harmala.

关 键 词：骆驼蓬草 骆驼蓬碱 去氢骆驼蓬碱 鸭嘴花碱 乙酰胆碱脂酶 薄层色谱生物自显影法 高效液相色谱 质量标准 

分 类 号：R29[医药卫生—民族医学]