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  

Simultaneous determination of linalool and protocatechuate in Homalomena occulta by quantitative nuclear magnetic resonance(qNMR)spectroscopy

作　　者：蒋丽娟 韦佳先 周平秀 张凤兰 张夏雯 李业航 JIANG Li-juan;WEI Jia-xian;ZHOU Pin-xiu;ZHANG Feng-lan;ZHANG Xia-wen;LI Ye-hang(School of Chemistry and Chemical Engineering,Guangxi Minzu University,Guangxi Key Laboratory for Polysaccharide Materials and Modification,Guangxi Higher Education Institutes Key Laboratory for New Chemical and Biological Transformation Process Technology,Nanning 5300,China;Guangxi Minzu University Hospital,Nanning 5300,China)

机构地区：[1]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 [2]广西民族大学医院,南宁530006

出　　处：《药物分析杂志》2024年第6期946-951,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：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)。

摘　　要：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^(1)H-qNMR测量,其中吡嗪、芳樟醇、原儿茶酸的定量共振峰分别为δ 8.66、δ 5.85~5.95、δ 6.78~6.80。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。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,^(1)H-q NMR measurement was performed on a 400 MHz spectrometer.The quantitative resonance peaks of pyrazine,Linalool and protocatechuate wereδ8.66,δ5.90 andδ8.60,respectively.Results:The linear correlation coefficients of linalool and protocatechuate were good with r of 0.9997 and 0.9986,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 detection 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 ^(1)H-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.

关 键 词：千年健 芳樟醇 原儿茶酸 氢核磁共振 多指标 质量评价 

分 类 号：R917[医药卫生—药物分析学]