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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(4.6mm×250mm,5μm),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1.0mL/min;进样量为20μL;豨莶苷、奇壬醇和豨莶精醇检测波长为215nm,防己诺林碱和粉防己碱检测波长为280nm。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6.45~129.00μg/mL(r=0.999 5)、5.61~112.20μg/mL(r=0.999 9)、4.25~85.00μg/mL(r=0.999 3)、9.19~183.80μg/mL(r=0.999 8)和11.05~221.00μg/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。
OBJECTIVE To establish a gradient elution combined with wavelength-switching HPLC method for the simultaneous determination of acetophenone, phenanthrolide, epigallocatechin, epirubicin and tetrandrine in Shuifeng and Rheumatism pill. Methods The gradient elution was performed on a Kromasil C18 column (4.6 mm × 250 mm, 5 μm) using mobile phase A: acetonitrile-methanol (2: 1) and mobile phase B: 0.05% glacial acetic acid at a flow rate of 1.0 mL / Injection volume of 20μL; carbendazim, odd nonyl alcohol and sperm alcohol detection wavelength of 215nm, anti-tubulin and tetrandrine detection wavelength of 280nm. Results The linear range of the concentrations of benatridine, cinannol, fenvalerate, nandroprine and tetrandrine were 6.45 ~ 129.00 μg / mL (r = 0.999 5), 5.61 ~ 112.20 μg (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) The average recoveries and relative standard deviations (RSDs) were 98.73% (1.43%), 97.63% (1.28%), 99.44% (1.29%), 98.33% (1.38%) and 97.36% (1.37% ). Conclusions The established gradient elution combined with wavelength-switching HPLC method can simultaneously determine the contents of benazid, cinanonol, fenugreek alcohol, tragernoline and tetrandrine in Shuifeng and Rheumatism pill. The method is simple, accurate and reproducible Good, provides a reliable method for Qionglai rheumatism pill quality control.