首页|定量核磁共振氢谱法同时测定千年健中芳樟醇、原儿茶酸的含量

定量核磁共振氢谱法同时测定千年健中芳樟醇、原儿茶酸的含量

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目的:采用氢核磁定量方法快速测定千年健中主要成分芳樟醇、原儿茶酸的含量.方法:以氘代二甲基亚砜为测试溶剂,吡嗪为内标物,在400 MHz光谱仪上进行1H-qNMR测量,其中吡嗪、芳樟醇、原儿茶酸的定量共振峰分别为δ8.66、δ5.85~5.95、δ6.78~6.80.结果:芳樟醇、原儿茶酸的线性关系良好,相关系数分别为0.999 7、0.998 5,精密度RSD分别为0.30%、0.40%,回收率分别为98.8%~100.7%(RSD为3.7%)和99.4%~100.6%(RSD为4.4%),表明所建立的氢核磁定量方法,结果准确,稳定可行,且整个检测过程在3 min左右完成.4批千年健药材中芳樟醇、原儿茶酸的含量范围分别为0.328~0.398 mg·g-1、0.559~0.630 mg·g-1.结论:该方法操作简单,分析速度快,专属性强,可用于千年健中2个有效成分的同步测定,为千年健药材的全面质量评价和质量控制提供科学依据.
Simultaneous determination of linalool and protocatechuate in Homalomena occulta by quantitative nuclear magnetic resonance(qNMR)spectroscopy
Objective:To establish a hydrogen nuclear magnetic quantitative method which can rapidly determine the contents of linalool and protocatechuate in Homalomena occulta.Methods:Using dimethyl sulfoxide-d6(DMSO-d6)as the test solvent and pyrazine-as the internal standard,1H-q NMR measurement was per-formed on a 400 MHz spectrometer.The quantitative resonance peaks of pyrazine,Linalool and protocatechuate were δ8.66,δ5.90 and δ8.60,respectively.Results:The linear correlation coefficients of linalool and proto-catechuate were good with r of 0.999 7 and 0.998 6,respectively.The RSDs of precision were 0.30%and 0.40%,and the recoveries were 98.8%-100.7%(RSD=3.7%)and 99.4%-100.6%(RSD=4.4%),respectively,which indicated that the established method was accurate,stable and feasible.And the whole detec-tion process was completed in about three minutes.The contents of 2 components in 4 batches of Homalomena occulta were 0.328-0.398 mg·g-1(linalool)and 0.559-0.630 mg·g-1(protocatechuate),respectively.Conclusion:The 1H-q NMR method has the advantages of simple operation,fast analysis speed and specificity,and can be used for the simultaneous determination of two active components in Homalomena occulta,providing a scientific basis for the overall quality evaluation and quality control of Homalomena occulta.

Homalomena occultalinaloolprotocatechuate1H-qNMRmulti-indexquantitative evaluation

蒋丽娟、韦佳先、周平秀、张凤兰、张夏雯、李业航

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广西民族大学化学化工学院,广西多糖材料与改性重点实验室,广西高校化学与生物转化过程新技术重点实验室,南宁 530006

广西民族大学医院,南宁 530006

千年健 芳樟醇 原儿茶酸 氢核磁共振 多指标 质量评价

广西民族大学2023年实验技术创新与实验室管理研究项目

2023MDSY003

2024

药物分析杂志
中国药学会

药物分析杂志

CSTPCD北大核心
影响因子:1.039
ISSN:0254-1793
年,卷(期):2024.44(6)