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目的:建立玉屏风散多波长、多成分含量测定的HPLC方法。方法:采用YMC Hydrosphere C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈(A)-0.05%磷酸水溶液(B),梯度洗脱,流速为1.0 mL·min~(-1),柱温为30℃,检测波长300 nm(升麻素苷)、257 nm(毛蕊异黄酮葡萄糖苷)、246 nm(升麻素)、294 nm(5-O-甲基维斯阿米醇苷)、256 nm(亥茅酚苷)、248 nm(毛蕊异黄酮)、249 nm(芒柄花素)、221 nm(白术内酯Ⅲ)、220 nm(白术内酯Ⅰ)、278 nm(白术内酯Ⅱ)。结果:在所建立色谱条件下各成分的专属性良好,无干扰峰;线性关系良好,均在0.999 5以上;仪器精密度(n=6)的RSD均小于2%;方法重复性(n=6)的RSD均小于2%;48 h内稳定,RSD均小于2%;回收率在98%~100%,RSD均小于2%,回收率较佳。测得升麻素苷、毛蕊异黄酮葡萄糖苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、毛蕊异黄酮、芒柄花素、白术内酯Ⅲ、白术内酯Ⅰ、白术内酯Ⅱ的含量平均值分别为0.032%、0.022%、0.012%、0.038%、0.004%、0.009%、0.006%、0.006%、0.005%、0.004%。结论:经方法学验证,本法可在同一色谱条件下利用不同检测窗口实现多类组分及多个成分的同时测定。
OBJECTIVE: To establish HPLC method for determination of multi-wavelength and multi-component content of Yupingfeng San. Methods: The mobile phase consisted of acetonitrile (A) - 0.05% phosphoric acid solution (B) with gradient elution on a YMC Hydrosphere C 18 column (4.6 mm × 250 mm, 5 μm) with a flow rate of 1.0 mL · min ~ 1), the column temperature was 30 ℃, the detection wavelength was 300 nm (ciclogram), 257 nm (calycosin), 246 nm (ciliminase), 294 nm (Atolinogen), 248 nm (calomel), 249 nm (atorchin), 221 nm (atractylosin III), 220 nm Atractylolide II). Results: Under the established chromatographic conditions, each component had good specificity and no interference peaks; the linearity was good, all above 0.999 5; RSD of instrument precision (n = 6) was less than 2% 6) showed stable RSD less than 2% within 48 h and RSD less than 2%. The recoveries ranged from 98% to 100% with RSD less than 2%. Measured cinnabarin, calycosin glucoside, cimicifuga, 5-O-methylWestainin, glucosinolates, Calendula officinalis, Ⅰ, the average content of atractyloside Ⅱ is 0.032%, 0.022%, 0.012%, 0.038%, 0.004%, 0.009%, 0.006%, 0.006%, 0.005%, 0.004% respectively. Conclusion: This method can be used for the simultaneous determination of multiple components and multiple components under different chromatographic conditions under the same chromatographic conditions.