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。 |
关键词: 高效液相色谱法 梯度洗脱联合波长切换 豨莶风湿丸 豨莶苷 奇壬醇 豨莶精醇 防己诺林碱 粉防己碱 |
DOI:10.16781/j.0258-879x.2016.12.1564 |
投稿时间:2016-05-25修订日期:2016-07-12 |
基金项目: |
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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 |
WEI Kun-xuan1,LUO Jun1*,LIU Guo-ping1,XU Jia-jia2 |
(1. Department of Pharmacy, the First Affiliated Hospital of Guangxi Medical University, Nanning 530021, Guangxi, China; 2. School of Pharmaceutical Science, Guangxi Medical University, Nanning 530021, Guangxi, China * Corresponding author) |
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. |
Key words: high performance liquid chromatography gradient elution joint wavelength switching Xixian Fengshi Wan darutoside kirenol darutigenol fangchinoline tetrandrine |