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机构地区:[1]杭州市中医院中药实验室,浙江杭州310007
出 处:《中华中医药学刊》2012年第2期330-332,共3页Chinese Archives of Traditional Chinese Medicine
基 金:浙江省科技计划资助项目(2009C33100)
摘 要:目的:建立高效液相色谱法测定活血止痛膏中芍药苷、马钱子碱、士的宁的含量。方法:采用AgilentTC-C18色谱柱(250 mm×4.6 mm,5μm),柱温为25℃,流速为1 mL.min-1;芍药苷的流动相为乙腈-水(16∶84),检测波长为230 nm;马钱子碱、士的宁的流动相为乙腈-0.01mol.L-1庚烷磺酸钠与0.02mol.L-1磷酸二氢钾等量混合溶液(用10%磷酸溶液调节pH值至2.8)(21∶79),检测波长为260 nm。结果:两种液相方法可分别测定活血止痛膏中芍药苷、马钱子碱、士的宁的含量。芍药苷浓度在25.2~200.2μg.mL-1(r=0.9996),马钱子碱浓度在2.45~19.6μg.mL-1(r=0.9998),士的宁浓度在2.95~23.6μg.mL-1(r=0.9997)范围内与其峰面积呈良好的线性关系;平均回收率(n=9)分别为95.13%(RSD=1.77%),87.63%(RSD=2.99%),90.93%(RSD=2.57%)。结论:两种液相测定方法专属性强,结果准确,可用于活血止痛膏的质量控制。Objective: To establish an HPLC method to determine the contents of peoniflorin, brucine and strychnine in Huoxue Zhitong Plaster. Mthod: Agiltnt C18 was employed. The column temperature was 25 ℃ and the flow rate was 1 mL · min^-1. Acetonitrile-water( 16:84) was adopted as the mobile phase of peoniflorin and the UV detection wavelength was 230nm. A mixture of acetonitrile and a mixture solution of equal quantities of 0.01mol · L-1 sodium heptane- sulfonate and 0.02mol · L-1potassium dihydrogen phosphate (adjust pH to 2.8 with 10% phosphoric acid) (20 : 80) were adopted as the mobile phase of brucine, strychnine and the UV detection wavelength was 260nm. Result : The contents of three components could be determined respectively by two HPLC methods. The calibration curves were linear in the ranges of 25.2 - 200.21μg.mL-1 ( r = 0. 9996 ) for peoniflorin, 2.45 - 19.6 μg.mL-1 ( r = 0. 9998 ) for brucine, 2.95 - 23.6μg.mL-1 (r = 0. 9997) for strychnine. The average recoveries ( n = 9) of peoniflorin, brucine and strychnine were 95.13% ( RSD = 1.77% ) ,87.63% ( RSD = 2.99% ) ,90.93% ( RSD = 2.57% ) respectively. Conclusion : The two methods were accurate with good reproducibility and strong specificity. They were suitable for determination of three compounds in Huoxue Zhitong Plaster.
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