梯度洗脱联合波长切换HPLC法同时测定豨莶风湿丸中的豨莶苷、奇壬醇、豨莶精醇、防己诺林碱和粉防己碱
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广西医科大学第一附属医院,广西医科大学第一附属医院,广西医科大学第一附属医院,广西医科大学药学院

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Simultaneous determination of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wan by joint wavelength switching HPLC gradient elution method
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The First Affiliated Hospital of Guangxi Medical University,Guangxi Nanning,The First Affiliated Hospital of Guangxi Medical University,Guangxi Nanning,The First Affiliated Hospital of Guangxi Medical University,Guangxi Nanning,School of Pharmaceutical Science,Guangxi Medical University,Guangxi Nanning

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    摘要:

    目的 建立梯度洗脱联合波长切换HPLC法同时测定豨莶风湿丸中豨莶苷、奇壬醇、豨莶精醇、防己诺林碱和粉防己碱。方法 采用Kromasil C18色谱柱(4.6 mm×250 mm,5 μm),以流动相A:乙腈-甲醇(2:1)、流动相B:0.05%冰醋酸溶液进行梯度洗脱;流速为1.0 mL/min;进样量为20 μL;豨莶苷、奇壬醇和豨莶精醇检测波长为215 nm,防己诺林碱和粉防己碱检测波长为280 nm。结果 豨莶苷、奇壬醇、豨莶精醇、防己诺林碱和粉防己碱在给定浓度范围内的线性范围分别为6.45~129.00 μg/mL(r=0.999 5)、5.61~112.20 μg/mL(r=0.999 9)、4.25~85.00 μg/mL(r=0.999 3)、9.19~183.80 μg/mL(r=0.999 8)和11.05~221.00 μg/mL(r=0.999 7),线性关系良好;平均加样回收率和相对标准偏差(RSD)值分别为98.73%(1.43%)、97.63%(1.28%)、99.44%(1.29%)、98.33%(1.38%)、97.36%(1.37%)。结论 建立的梯度洗脱联合波长切换HPLC法能同时测定豨莶风湿丸中豨莶苷、奇壬醇、豨莶精醇、防己诺林碱和粉防己碱含量,方法简便、准确、重现性好,为豨莶风湿丸质量控制提供了可靠方法。

    Abstract:

    Objective To establish a joint wavelength switching HPLC gradient elution method for simultaneous determination of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wan. Methods A Kromasil C18 column (4.6 mm×250 mm, 5 μm) was used with a mobile phase A:acetonitrile-methano (2:1) and mobile phase B:0.05% acetic acid solution with gradient elution. The flow rate was 1.0 mL/min; the injection volume was 20 μL; darutoside, kirenol and darutigenol were detected at 215 nm, and fangchinoline and d-tetrandrine were detected at 280 nm. Results In the given concentration range, the linearity ranges of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine were 6.45-129.00 μg/mL (r=0.999 5), 5.61-112.20 μg/mL (r=0.999 9), 4.25-85.00 μg/mL (r=0.999 3), 9.19-183.80 μg/mL (r=0.999 8), and 11.05-221.00 μg/mL (r=0.999 7), respectively; and their average recoveries and RSD were 98.73% (1.43%), 97.63% (1.28%), 99.44% (1.29%), 98.33% (1.38%), and 97.36% (1.37%), respectively. Conclusion The established joint wavelength switching HPLC gradient elution method is simple, accurate and reproducible; it can simultaneously determine the contents of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wan and can be used for quality control of Xixian Fengshi Wan.

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  • 收稿日期:2016-05-25
  • 最后修改日期:2016-07-12
  • 录用日期:2016-09-26
  • 在线发布日期: 2016-12-23
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