HPLC-RID法替代滴定法测定百令胶囊中甘露醇含量的研究

Research on determination of mannitol in Bailing capsules by HPLC- RID instead of titration

目的：建立HPLC-RID法测定百令胶囊中甘露醇的含量。方法：样品以乙醇为溶剂，加热回流提取甘露醇。采用氨基柱（250 mm×4.6 mm，5 μm），以乙腈-水（86：14）为流动相，流速1.0 mL·min^-1，采用示差折光检测器进行检测。结果：甘露醇浓度在0.28～7.00 μg范围内，与色谱峰面积积分值呈良好线性关系，定量限8.55 μg，回收率在98.81%（n=6）。测定了3批样品，甘露醇含量范围为5.9～7.3 mg·粒^-1。结论：本方法简单、准确，专属、灵敏，适用于百令胶囊中甘露醇的含量测定；可以替代百令胶囊及其他发酵虫草制剂标准采用的，以测定含羟基化合物总量为甘露醇含量的氧化还原滴定法。

Objective： To establish an accurate HPLC-RID method for the determination of mannitol in Bailing capsules. Methods： Sample was extracted with ethanol by heating under reflux.Separation was achieved on a NH2 column （250 mm×4.6 mm,5 μm）,with acetonitrile-water （86： 14） as mobile phase and a flow rate at 1.0 mL· min^-1. Results： The contents of mannitol ranged from 5.9 to 7.3 mg per capsule in Bailing capsules.The linear range of mannitol was 0.28-7.00 μg,and the limit of quantification was 8.55 μg.The average recovery was 98.81%（n=6）. Conclusion： The method is simple,accurate,specific,sensitive and suitable for the determination of mannitol in Bailing capsules,and can be used as an alternative method to the redox titration adopted by the standards for Bailing capsules and other fermented Cordyceps preparations to measure the total amount of hydroxyl compound mannitol content.