维药骆驼蓬子药材质量标准研究  

Research on Quality Specification of the Seeds of Peganum harmala L. of A Uygur Traditional Medicine

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

机构地区：[1]上海中医药大学中药研究所,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,乌鲁木齐830011 [3]新疆医科大学药学院药剂物化教研室,乌鲁木齐830011

出　　处：《中国药学杂志》2014年第2期106-112,共7页Chinese Pharmaceutical Journal

基　　金：国家自然基金-新疆联合基金重点项目(U1130303);国家自然科学基金资助项目(81173119);国家"重大新药创制"科技重大专项(2012ZX0910320-051);上海市优秀学术带头人计划(13XD1403500);国家药典委员会2010药典标准提高项目(508)

摘　　要：摘要：目的建立骆驼蓬子药材的质量标准。方法参照2010年版《中国药典》附录相关方法，对骆驼蓬子水分、总灰分、酸不溶性灰分、50％乙醇浸出物和重金属进行检测。采用硅胶HSGF。薄层板，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、365nm）下检视、碘化铋钾显色及乙酰胆碱酯酶生物自显影技术对骆驼蓬子进行鉴别。采用C18色谱柱，以乙腈一醋酸铵缓冲盐（19：81）为流动相，检测波长为330nm，建立骆驼蓬子中去氢骆驼蓬碱（HAR）和骆驼蓬碱（HAL）的定量分析方法；以相同流动相梯度洗脱，检测波长为280nm，流速为0．7mL·min-1，建立骆驼蓬子药材特征图谱。结果采用紫外光（254、365nm）下检视、碘化铋钾显色及生物自显影技术联合分析可鉴别骆驼蓬子中的活性生物碱类成分。骆驼蓬碱和去氢骆驼蓬碱分别在1．97—198．68和1．70～345．30I,zg·mL“内呈良好的线性关系，平均回收率分别为99．69％（RSD为1．89％）和100．66％（RSD为1．78％）。11批骆驼蓬子药材中去氢骆驼蓬碱和骆驼蓬碱平均含量分别为3．76％和3．23％。在特征图谱中确定了4个峰为特征峰。结论药材中水分、总灰分、酸不溶性灰分、体积分数50％乙醇浸出物分别不得过9．0％、8．0％、1．0％和22．0％。重金属铅、镉、砷、汞、铜分别不得过5×10^-6、3×10^-6、2×10^-6、2×10^-6和20×10^-6。骆驼蓬碱和去氢骆驼蓬碱的含量总和限度不得低于5．5％。以骆驼蓬碱为参照物峰，特征图谱中4个特征峰的相对保留时间应在各规定值的±5％之内。建立的定性和定量方法可用于骆驼蓬子药材的质量控制。OBJECTIVE To develop the quality specification of seeds of Peganum harmala. METHODS According to the Chi- nese Pharmacopoeia （2010 Version, Volume 1） and its appendix method, the water, total ash, acid insoluble ash, 50% ethanol ex- tractives, and heavy metal were analyzed for seeds of P. harmala. TLC method was used to separate harmaline （ HAL ） , harmine （HAR） and vasicine （VAS） in seed samples using mixture of ethyl acetate-methanol-ammonia water （ 10： 1.5： 0. 5 ） as a developing solvent on high performance silica G pre-coated plate with 254 nm fluorescent （ GFa54 ） and to identify them inspected under UV 366 nm, 254 nm, visualized by spraying with both Dragendorff reagent and by bioautographie assay. In the HPLC method, HAL and HAR were separated on a Ct8 column with acetonitrile-ammonium acetate water （ 19：81 ） as the mobile phase and detected at 330 nm. The HPLC fingerprints were performed on the same CI8 column and eluted by using a linear gradient of acetonitrile （A） and 0. 1 mmol ·L- 1 ammonium acetate buffer under the flow rate at 0.7 mL·min - 1 and detected at 280 nm. RESULTS In the TLC procedures, 254 and 366 nm fluorescent, Dragendorff reagent, and bioautographic assay for the detection of acetylcholinesterase inhibitor can be used for qualitative identification of the active ingredients. For the HPLC quantitative method, the calibration curve of HAR displayed ideal linearity over the range of 1.97 - 198.68μg· mL - l with average recovery of 99. 69% （ RSD of 1.89% ）. HAL displayed ideal linearity over the range of 1.70 -345.30 μg· mL-lwith average recovery of 100. 66% （RSD of 1.78% ）. The contents of HAL and HAR in11 batches of seeds of P. harmala were 3. 234% and 3. 755%. In the characteristic fingerprints of seeds of P. harmala, four common peaks were identified. CONCLUSION The results indicated that the water, total ash, acid insoluble ash, and 50% ethanol extrac- tives were not more than 9.0% , 8.0% , 1.0% , and 22. 0% , respectively. The heavy

关 键 词：骆驼蓬子 骆驼蓬碱 去氢骆驼蓬碱 鸭嘴花碱 高效液相色谱法 特征图谱 薄层色谱-生物自显影法 乙酰胆碱酯酶抑 制剂 质量标准 

分 类 号：R284[医药卫生—中药学]