HPLC法测定不同地区制川乌中新乌头碱、次乌头碱及乌头碱含量.docVIP

HPLC法测定不同地区制川乌中新乌头碱、次乌头碱及乌头碱含量摘要：目的测定制川乌不同炮制品中新乌头碱、次乌头碱及乌头碱的含量。方法采用HPLC法，色谱柱为Kromasil-C18柱，甲醇-水-氯仿-三乙胺（体积比70∶30∶2∶0.1）为流动相，流速1.0 mL/min，检测波长230 nm，柱温为常温。结果新乌头碱在0.025～0.3 mg/mL，乌头碱在0.01～0.117 mg/mL，次乌头碱在0.025～0.3 mg/mL范围内线性关系良好，平均回收率分别为97.3 %，98.1 %，96.8 %。结论制川乌中酯型生物碱含量均不超过0.15%，符合中国药典规定。 关键词：制川乌；生物碱；含量测定 中图分类号：R282.71文献标识码：A文章编号：1672-979X(2008)09-0044-03 Determinations of Mesaconitine, Hypaconitine and Aconitine in Radix Aconiti preparata from Different Areas by HPLC ZHU Jun-fang, LI Zhuo-ya, SHEN Zhi-bin*, JIANG Yong-he, YUAN Ji-cheng (Guangdong Pharmaceutical University, Guangzhou 510006, China) Abstract：Objective To determine the contents of mesaconitine, hypaconitine and aconitine in different processed products of Radix Aconiti preparata. Methods A HPLC method was established on a Kromasil C18 column with the mobile phase consisting of methanol-water- chloroform- triethylamine(70∶30∶2∶0.1) and flow rate of 1.0 mL/min at common temperature. The detection wavelength was 230 nm. Results The calibration curves showed good linearity in the range of 0.025～0.3 mg/mL of mesaconine, 0.01～0.117 mg/mL of aconitine and 0.025～0.3 mg/mL of hypaconine, respectively. And the average recoveries for mesaconine, aconitine and hypaconine were 97.3 %, 98.1 % and 96.8 %, respectively. Conclusion The content of ester alkaloids does not surpass 0.15 % in Radix Aconiti preparata, which conforms to the requirement of Chinese Pharmacopoeia. Key words：Radix Aconiti preparata; alkaloid; assay 制川乌为川乌的炮制加工品，含有多种生物碱，其中主要有新乌头碱、次乌头碱及乌头碱。现有文献多测定制川乌中1种或2种生物碱含量，同时测定3种生物碱含量的文献报道较少。我们研究了不同地区的制川乌，测定了新乌头碱、次乌头碱及乌头碱的含量，以期为制川乌生产的规范化、饮片生产的标准化提供依据。 1仪器与试药 Waters 515 型高效液相色谱仪（Waters 515泵，2487紫外检测器，EmPower色谱工作站) ；乌头碱（批号110720-200410）、次乌头碱（批号0798-9403）、新乌头碱（批号0799-9403）等对照品均购自中国药品生物制品检定所；甲醇、氯仿为色谱纯，余为分析纯；水为重蒸馏水。 制川乌饮片来源见表1，经广东药学院生药教研室李书渊副教授鉴定。 2方法和结果 2.1色谱条件[1] 色谱柱：Kromasil C18（250 mm×4.6 mm，5 μm)，流动相：甲醇-水-氯仿-三乙胺（70∶30∶2∶0.1）；流速：1.0 mL/min；检测波长：230 nm；柱温：室温。 2.2溶液的制