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作 者:陶健 TAO Jian(Department of Pharmacy, Pingdingshan Hospital of Traditional Chinese Medicine, Pingdingshan 467099, Chin)
机构地区:[1]平顶山市中医医院药学部,河南平顶山467099
出 处:《实用药物与临床》2018年第5期564-568,共5页Practical Pharmacy and Clinical Remedies
摘 要:目的建立高效液相波长切换法同时测定芪归通便合剂中6种成分的含量。方法采用Diamonsil C18色谱柱(250 mm×4.6 mm,5μm);以甲醇-乙腈(1∶1)与0.1%甲酸溶液为流动相,梯度洗脱;流速0.8 m L/min;柱温30℃。结果松果菊苷、毛蕊花糖苷、毛蕊异黄酮葡萄糖苷、芒柄花素、白术内酯Ⅲ、白术内酯Ⅰ6个成分在12.09~241.80μg/m L(r=0.999 2)、5.51~110.20μg/m L(r=0.999 5)、2.55~51.00μg/m L(r=0.999 8)、3.94~78.80μg/m L(r=0.999 1)、2.08~41.60μg/m L(r=0.999 9)、1.91~38.20μg/m L(r=0.999 4)范围内,与峰面积线性关系良好;平均加样回收率(RSD)分别为99.47%(RSD=1.08%)、98.37%(RSD=1.54%)、96.99%(RSD=1.40%)、98.05%(RSD=0.88%)、98.70%(RSD=1.25%)、97.64%(RSD=0.98%)。结论本文建立的HPLC波长切换法同时测定芪归通便合剂中的6个成分含量,可作为芪归通便合剂全面可靠的质量控制方法。Objective To develop a high performance liquid chromatography method for determination of six components in Qiguitongbian Heji simultaneously. Methods The Diamonsil C18( 250 mm × 4. 6 mm,5 μm) chromatographic column was adopted; the mobile phase was methanol-acetonitrile( 1∶ 1) and 0. 1% formic acid solution with gradient elution,at a flow rate of 0. 8 m L/min,and the column temperature was set at 30 ℃. Results The linear response range of echinacoside,verbascoside,calycosin7-O-β-D-glucopyranoside,formononetin,atracylenolide Ⅲ and atracylenolideⅠ were 12. 09 - 241. 80 μg/m L( r = 0. 999 2),5. 51 - 110. 20 μg/m L( r = 0. 999 5),2. 55 - 51. 00 μg/m L( r = 0. 9998),3. 94 - 78. 80 μg/m L( r = 0. 999 1),2. 08 - 41. 60 μg/m L( r = 0. 999 9),and 1. 91 - 38. 20 μg/m L( r = 0. 999 4),respectively. The average recoveries and the corresponding RSD were 99. 47%( 1. 08%),98. 37%( 1. 54%),96. 99%( 1. 40%),98. 05%( 0. 88%),98. 70%( 1. 25%) and 97. 64%( 0. 98%),respectively. Conclusion This HPLC wavelength switching method has been successfully established for simultaneous determination of 6 components in Qiguitongbian Heji. The method is helpful for the quality control of Qiguitongbian Heji.
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