HPLC梯度洗脱法同时测定活血镇痛膏中防己诺林碱、粉防己碱、新乌头碱、乌头碱和次乌头碱  

Simultaneous Determination of Fangchinoline,Tetrandrine,Mesaconitine,Aconitine and Hypaconitine in Huoxue Zhentong Plaster by HPLC with Gradient Elution

作　　者：谭雄斯[1] 庞武耀[1] 

机构地区：[1]肇庆医学高等专科学校,广东肇庆526020

出　　处：《中国药师》2017年第4期763-765,共3页China Pharmacist

摘　　要：目的:建立同时测定活血镇痛膏中的防己诺林碱、粉防己碱、新乌头碱、乌头碱和次乌头碱含量的HPLC梯度洗脱法。方法:采用Dikma-C18色谱柱(200 mm×4.6 mm,5μm),以甲醇-乙腈(3∶1)(A)与0.06%二乙胺水溶液(B)为流动相,进行梯度洗脱,检测波长分别为280 nm(防己诺林碱和粉防己碱)、235 nm(新乌头碱、乌头碱和次乌头碱),流速1.0 ml·min^(-1),柱温30℃,进样量为10μl。结果:防己诺林碱、粉防己碱、新乌头碱、乌头碱和次乌头碱5个成分的质量浓度分别在7.490~149.800、14.610~292.200、4.150~83.000、5.250~105.000、5.140~102.800μg·ml^(-1)范围内呈良好线性关系,r分别为0.999 9,0.999 8,0.999 2,0.999 6,0.999 9;平均加样回收率(RSD)分别为99.87%(0.49%),97.79%(1.11%),96.97%(1.75%),98.60%(1.50%),97.94%(0.98%)(n=6)。结论:本文建立的HPLC梯度洗脱法能同时测定活血镇痛膏中的5个成分,该方法简便、稳定、可靠,可作为活血镇痛膏全面可靠的质量控制方法。Objective： To develop an HPLC gradient elution method for the simultaneous determination of fangchinoline, tetrandrine, mesaeonitine, aeonitine and hypaconitine in Huoxue Zhentong plaster. Methods： ：A Dikma-Cls （200 mm × 4.6mm, 5 μm） chromatographic column was adopted, the mobile phase was methanol-acetonitrile （3 ： 1 ） （A）-0.06% diaethylamin solution （B） with gradient elution at a flow rate of 1.0 ml · min^ -1, the detection wavelength was 280 nm for fangchinoline and tetrandrine, and 235 nm for mesaeonitine, aconitine and hypaconitine. The column temperature was set at 30℃, and the injection volume was 10 μl. Results： ：There was a good linear relationship when the content of fangchinoline, tetrandrine, mesaconitine, aconitine and hypaconitine was within the range of 7. 490-149. 800μg·ml^-1 （r = 0. 999 9 ）, 14. 610-292. 200μg·ml^-1 （r = 0.999 8 ）, 4. 150-83. 000 μg·ml^-1 （r = 0.999 2）, 5. 250-105. 000 μg·ml^-1 （ r = 0.999 6） and 5. 140-102.800 μg·ml^-1 （ r = 0. 999 9 ）, respectively. The average recovery and the corresponding RSD were 99.87% （0.49%） ,97.79% （ 1.11% ）, 96.97% （ 1.75% ） ,98.60% （ 1.50% ） and 97.94% （0.98 % ） （ n = 6 ）, respectively. Conclusion： An HPLC gradient elution method is successfully established for the simultaneous determination of 5 components in Huoxue Zhentong plaster. The established method is simple, accurate and reliable, which is helpful to the quality control of Huoxue Zhentong plaster.

关 键 词：活血镇痛膏 防己诺林碱 粉防己碱 新乌头碱 乌头碱 次乌头碱 梯度洗脱法 高效液相色谱法 梯度洗脱 

分 类 号：R927.2[医药卫生—药学]