HPLC Determination of 5-Hydroxymethylfurfural and Ecdysterone in Granules of Radix Achyranthis Bidentatae
摘 要
提出了高效液相色谱法同时测定牛膝配方颗粒中5-羟甲基糠醛和蜕皮甾酮的含量的方法。采用SHIMADZU shim-pack VP-ODS(4.6 mm ×250 mm,4.6 μm)柱;用两种不同配比的乙腈和水混合溶液作为流动相,梯度洗脱;检测波长为279 nm(5-羟甲基糠醛)和245 nm(蜕皮甾酮)。5-羟甲基糠醛和蜕皮甾酮的质量浓度分别在0.390~100 mg·L-1和3.125~100 mg·L-1范围内与峰面积呈线性关系,方法的检出限(3S/N)分别为1.95, 2.01 ng。5-羟甲基糠醛和蜕皮甾酮的平均回收率分别为99.7%,99.1%;相对标准偏差(n=5)分别为0.80%,0.67%。
Abstract
HPLC was applied to the simultaneous determination of 5-hydroxymethylfurfural and ecdysterone in granules of radix achyranthis bientatae for making up prescriptions. SHIMADZU shim-pack VP-ODS column (4.6 mm×250 mm, 4.6 μm) was used for separation. Mixtures containing acetonitrile and water mixed in different ratio were used as the mobile phase in gradient elution. UV-detection at the wavelengths of 279 nm (for 5-hydroxymethylfurfural) and 245 nm (for ecdysterone) was adopted in the determination. Linear relationships between values of peak area and mass concentration of 5-hydroxymethylfurfural and ecdysterone were obtained in the ranges of 0.390-100 mg·L-1 and 3.125-100 mg·L-1, with detection limits (3S/N) of 1.95 ng and 2.01 ng respectively. Results of recovery and precision found were: values of average recovery of 99.7% for 5-hydroxymethylfurfural and 99.1% for ecdysteronen with values of RSD′s (n=5) 0.80% and 0.67% respectively.
中图分类号 O652.63
所属栏目 工作简报
基金项目 河南省教育厅自然科学基金课题(2010A350003)
收稿日期 2011/3/11
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备注赵变(1985-),女,河南驻马店人,硕士研究生,主要从事色谱分析工作。
引用该论文: ZHAO Bian,GUO Hong-yun,CHANG Zhen-zhen,SUN Xiang-de. HPLC Determination of 5-Hydroxymethylfurfural and Ecdysterone in Granules of Radix Achyranthis Bidentatae[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(5): 580~582
赵变,郭红云,常珍珍,孙祥德. 高效液相色谱法测定牛膝颗粒中5-羟甲基糠醛和蜕皮甾酮的含量[J]. 理化检验-化学分册, 2012, 48(5): 580~582
被引情况:
【1】党建章,聂小忠,金刚,赵伟鑫,罗斌, "高效液相色谱法测定海带中3,5-二碘酪氨酸",理化检验-化学分册 51, 250-251(2015)
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参考文献
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【2】MICHAEL D, COURREUR T, LENAERTS V, et al. Effects of ecdysterone on the differentiation of normal human keratinocytesin vitro[J]. Eur J Dermatol, 1994,4(7):558-560.
【3】刘振丽,宋志前,王淳,等.泛糖程度不同的牛膝中5-羟甲基糠醛含量测定[J].中国中药杂志, 2009,34(3):298-300.
【4】梁生旺,王静,王淑美,等.牛膝“泛糖”机制研究[J].中草药, 2003,34(11):993-996.
【5】孟大利,侯柏玲,汪毅,等.中药牛膝中的植物甾酮类成分[J].沈阳药科大学学报, 2006,23(9):562-564.
【6】林大专,王广树,杨晓红,等.牛膝中新蜕皮甾酮类成分的研究[J].中国药学杂志, 2006,41(17):1295-1297.
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