HPLC-RID法替代滴定法测定百令胶囊中甘露醇含量的研究

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.

[1] ChP 2010.Vol Ⅰ(中国药典2010年版.一部)[S].2010:681
[2] XIAO Xin-yue(肖新月),LI Yuan-ke(李远科),ZHANG Ping(张萍),et al.RP-HPLC determination of nucleosides in Ningxinbao capsules(宁心宝胶囊中5种核苷类成分的RP-HPLC定量分析)[J].Chin J Pharm Anal(药物分析杂志),2007,27(10) :1592
[3] CHENG Xian-long(程显隆),XIAO Xin-yue(肖新月),ZOU Qin-wen(邹秦文),et al.Pre-column derivatization HPLC simultaneous determination of 4 main amino acids in donkey-hide glue(柱前衍生化HPLC法同时测定阿胶中4种主要氨基酸的含量)[J].Chin J Pharm Anal(药物分析杂志),2008,28(12):1997
[4] ZOU Qin-wen(邹秦文),XIAO Xin-yue(肖新月),CHENG Xian-long(程显隆),et al.Pre-column derivatization RP-HPLC determination of 17 amino acids in Bailing capsules(百令胶囊中17种氨基酸的柱前衍生化RP-HPLC法含量测定)[J].Chin J Pharm Anal(药物分析杂志),2010,30(9):1630
[5] CHEN Yi-jian(陈毅坚),ZHANG Zhuo(张灼).Internal standard method for the determination of mannitol in Cordyceps sinensis by high performance liquid chromatography(示差折光检测-高效液相色谱内标法测定虫草中的甘露醇)[J].Chin J Spect Lab(光谱实验室),2004,21(3):492
[6] SHI Yan-zhi(施燕支),GUO Xue-qing(郭雪清),YU Qi-rong(余启荣),et al.Determination of many kinds of components in chewing gum by HPLC with refractive index detector(HPLC示差折光分析法测定口香糖中的木糖醇等多种糖醇的含量)[J].J Cap Norm Univ(首都师范大学学报),2005,26(1):61
[7] DONG Xiao-dong(董晓东),HOU Wan-ling(侯宛玲),SU Shao-zhe(苏绍哲).Determination of glucose and mannitol by HPLC(高效液相色谱法测定葡萄糖和甘露醇)[J].Chin J Anal Chem(分析化学),2000,28(5):656
[8] ZHAO Lian-chao(赵联朝),DONG Zheng-rong(董正荣).Maintenance and Analytical Instrument(分析仪器及维护)[M].Beijing(北京):China Environmental Science Press(中国环境科学出版社),2007
[9] WEI Feng(魏锋),WU Zhao-yang(吴朝阳),MA Ling-yun(马玲云),et al.RP-HPLC-RID determination of fructooligosaccharides in Chinese medicine and functional foods(RP-HPLC-RID测定中药和保健食品中低聚果糖的含量)[J].Asia-Pac Tradit Med(亚太传统医药),2009,5(9):20
[10] LIANG Wei-yang(粱蔚阳),FENG Wei-jing(冯炜菁).Determination of fructose and glucose in invert sugar for injection by HPLC-RID(高效液相色谱-示差折光检测法测定注射用转化糖中果糖与葡萄糖的含量)[J].Chin J Biochem Pharm(中国生化药物杂志),2007,28(2):116
[11] TIAN Zhen-le(田贞乐),XU Chun-hua(徐春花),ZHENG Hui- hua(郑惠华),et al.Determination of mannitol in mycelium of Cordyceps sinensis by HPLC-RID(HPLC-RID法测定虫草菌丝体中甘露醇)[J].Acta Edulis Fungi(食用菌学报),2010,17 :113
[12] ZHANG Ying(张英),SHI Xue-ping(石雪萍),ZHANG Wei- ming(张卫明).Comparison of HPLC-ELSD and HPLC-RID methods in detecting the sugar of honey(HPLC-ELSD法与HPLC-RID法检测蜂蜜中糖分的比较)[J].Chin Wild Plant Res(中国野生植物资源),2009,28(1):43