摘要
目的 建立通窍鼻炎片(Tongqiao Biyan tablets,TBT)的HPLC指纹图谱及对升麻素苷、5-O-甲基维斯阿米醇苷、毛蕊异黄酮葡萄糖苷、欧前胡素、异欧前胡素、白术内酯Ⅰ6个指标成分的定量分析方法.方法 采用AlltimaTM C18色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.2％甲酸溶液为流动相进行梯度洗脱,检测波长254 nm.利用中药色谱指纹图谱相似度评价系统建立TBT对照指纹图谱,并进行相似度评价.同时对通窍鼻炎片中升麻素苷、5-O-甲基维斯阿米醇苷、毛蕊异黄酮葡萄糖苷、欧前胡素、异欧前胡素及白术内酯Ⅰ6个指标成分进行含量测定.结果 建立的TBT对照指纹图谱中,共匹配出10个共有峰,通过对照品指认了其中6个指标成分:升麻素苷(1号峰)、毛蕊异黄酮葡萄糖苷(2号峰)、5-O-甲基维斯阿米醇苷(4号峰)、欧前胡素(7号峰)、异欧前胡素(8号峰)和白术内酯Ⅰ(10号峰),相似度介于0.991～0.998.上述6个成分分别在 0.051～0.605 4 μg(R2=0.999 2)、0.008 2～0.327 3 μg(R2=0.999 3)、0.014 3～0.570 3 μg(R2=1.000 0)、0.030 7～1.228 8 μg(R2=1.000 0)、0.014 7～0.589 7 μg(R2=1.000 0)、0.002 3～0.091 8 μg(R2=1.000 0)范围内与峰面积线性关系良好,平均加样回收率为96.4％～102.2％,RSD均小于3.0％(n=9),精密度、稳定性、重复性试验RSD均小于3.0％.结论 所建立的HPLC指纹图谱及含量测定方法稳定、可控,适用于通窍鼻炎片的质量控制.
Abstract
Objective To establish an HPLC fingerprint of Tongqiao Biyan tablets(TBT)and a quantitative analysis method for six components including cimicifugoside,5-O-Methylvisammioside,Calycosin-7-O-beta-D-glucoside,Imperatorin,Isoimperatorin,and Atractylenolide-Ⅰ.Methods The AlltimaTM C18 column(250 mum × 4.6 mm,5 μm)was used with acetonitrile-0.2％formic acid solution as the mobile phase for gradient elution,and the detection wavelength was set at 254 nm.The TBT reference fingerprint was established using the similarity evaluation system of traditional Chinese medicine chromatographic fingerprints,and the similarity was evaluated.The contents of the six marker components were determined in Tongqiao Biyan tablets.Results In the established TBT reference fingerprint,a total of 10 common peaks were matched,and six marker components were identified using reference sub-stances:cimicifugoside(peak 1),calycosin-7-O-beta-D-glucoside(peak 2),5-O-methylvisammioside(peak 4),imperatorin(peak 7),isoimperatorin(peak 8),and atractylenolide-Ⅰ(peak 10),with similarity ranging from 0.991 to 0.998.The linear relationships between the peak area and the amount of the six components were good within the ranges of 0.051-0.605 4 μg(R2=0.999 2),0.008 2-0.327 3 μg(R2=0.999 3),0.014 3-0.570 3 μg(R2=1.000 0),0.030 7-1.228 8 μg(R2=1.000 0),0.014 7-0.589 7 μg(R2=1.000 0),and 0.002 3-0.091 8 μg(R2=1.000 0),respectively.The average recovery rates were 96.4％-102.2％,with RSD less than 3.0％(n=9),and the precision,stability,and repeatability RSDs were all less than 3.0％.Conclusion The estab-lished HPLC fingerprint and the content determination method are stable and controllable,suitable for the quality control of Tongqiao Biyan tablets.
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