HPLC-一测多评法测定黄精及其饮片中6种成分的含量
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篇名: HPLC-一测多评法测定黄精及其饮片中6种成分的含量
TITLE:
摘要: 目的:建立黄精及其饮片中薯蓣皂苷元、5-羟甲基糠醛、香草酸、芦丁、槲皮素及山柰酚6种成分的一测多评(QAMS)法。方法:采用高效液相色谱(HPLC)外标法同时测定黄精及其饮片中6种成分的含量[色谱柱为Diamonsil-C18;流动相为乙腈-水(梯度洗脱);5-羟甲基糠醛、香草酸、芦丁、槲皮素及山柰酚检测波长为254 nm(0~60 min),薯蓣皂苷元检测波长为202 nm(60~75 min);流速为1.0 mL/min;柱温为30 ℃]。以香草酸为内标,分别计算出其余5种成分的相对校正因子(RCFs)并进行耐用性考察,并采用相对保留法对待测成分色谱峰进行准确定位,然后根据RCFs计算黄精药材中其他5种成分的含量,并与外标法测定结果进行比较。以黄精饮片进行方法验证,分别采用QAMS法和外标法测定其中6种成分的含量,比较两种方法含量测定差异。结果:HPLC方法学考察结果均符合相关要求。在线性范围内,薯蓣皂苷元、5-羟甲基糠醛、芦丁、槲皮素及山柰酚的RCFs分别为0.195、0.025、0.263、0.345、0.075,在不同试验条件下RCFs重现性良好。外标法和QAMS法两种方法测得的黄精药材及其饮片中6种成分的含量差异均无统计学意义(P>0.05)。结论:建立的QAMS法可用于同时测定黄精药材及其饮片中6种成分含量。
ABSTRACT: OBJECTIVE: To establish a quantitative analysis of multi-components by singer marker (QAMS) for determining the contents of diosgenin, 5-hydroxymethylfurfural, vanillic acid, rutin, quercetin, kaempferol in Polygonati Rhizoma and its decoction piece. METHODS: HPLC external standard method was used to determine the contents of 6 components in Polygonati Rhizoma and its decoction piece simultaneously [the separation was carried out on Diamonsil-C18 column with mobile phase consisted of acetonitrile-water (gradient elution); the detection wavelengths of 5-hydroxymethylfurfural, vanillic acid, rutin, quercetin and kaempferol were set at 254 nm(0-60 min); the detection wavelength of diosgenin was set at 202 nm (60-75 min) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃]. Using vanillic acid as internal standard, relative correction factors (RCFs) of aother 5 components were calculated and to investigate durability. Relative retention method was used to accurately locate the chromatographic peaks of the components to be determined, and then the contents of the aother 5 components in Polygonati Rhizoma were calculated according to RCFs, and the results were compared with those determined by external standard method. The method was validated by Polygonati Rhizoma decoction piece. The contents of 6 components were determined by QAMS method and external standard method respectively, and then the differences of content determination were compared between 2 methods. RESULTS: The methodology investigation results of HPLC method were in line with related requirements. Within the linear range, the RCFs of diosgenin, 5-hydroxymethylfurfural, rutin, quercetin, kaempferol were 0.195, 0.025, 0.263, 0.345 and 0.075, respectively. Under different experiment conditions, RCFs showed good reproducibility; there was no statistical significance of 6 components in Polygonati Rhizoma and its decoction piece determined by external standard method and QAMS method (P>0.05). CONCLUSIONS: Established QAMS method is suitable for simultaneous determination of 6 components in Polygonati Rhizoma and its decoction piece.
期刊: 2019年第30卷第13期
作者: 左雅敏,李琛,彭兴春,卫荣华,伍庆,郑燕,邓雪华
AUTHORS: ZUO Yamin,LI Chen,PENG Xingchun,WEI Ronghua,WU Qing,ZHENG Yan,DENG Xuehua
关键字: 一测多评法;黄精;饮片;质量控制;高效液相色谱法
KEYWORDS: Quantitative analysis of multi-components by singer marker; Polygonati Rhizoma; Decoction piece; Quality control; HPLC
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