Gansu Agricultural University, College of Agronomy, Gansu Provincial Key Laboratory of Arid Land Crop Science, Lanzhou 730070, People's Republic of China.
J AOAC Int. 2020 Nov 1;103(6):1633-1638. doi: 10.1093/jaoacint/qsaa054.
As known to us, HPLC method was often used to determine the contents of Angelicae sinesis Radix. In view of the shortcomings of HPLC method, qNMR has prominent advantages in determining the contents of bioactive components in the quantitative and qualitative analysis of Angelicae sinesis Radix.
In this study, a quick, simple, and accurate method was established to determine the components of ferulic acid, coniferyl ferulate, and ligustilide in Angelicae sinesis Radix.
Using dimethyl sulfoxide-d6(DMSO-d6) as the test solvent and pyrazine as the internal standard substance, 1H-qNMR measurement was performed on a 600 MHz spectrometer. The quantitative resonance peaks of pyrazine, ferulic acid, ligustilide, and coniferyl ferulate were at δ8.66 ppm, δ6.35-6.37 ppm, δ5.53-5.55 ppm, and δ6.50-6.53 ppm, respectively.
The linear relationship, limit of detection, limit of quantification, precision, stability, and recovery were verified and the results were good. On the other hand, it was verified by HPLC, and the HPLC used for verification passed the methodological investigation of linearity, precision, repeatability, stability, and recovery, and the results were good. In addition, no significant difference in results was found between the 1H-qNMR and HPLC-UV methods in determining the content of three components in three batches of Angelicae sinesis Radix.
The method can be used for simultaneous determination of three active components, and providing a scientific basis for the overall quality evaluation and quality control of Angelicae sinesis Radix.
In this study, 1H-qNMR was used to determine ferulic acid, coniferyl ferulate and ligustilide in Angelicae Sinensis Radix for the first time.
众所周知,高效液相色谱法常用于测定当归药材的含量。鉴于高效液相色谱法的缺点,定量核磁共振(qNMR)在当归的定量和定性分析中对生物活性成分的含量测定具有突出的优势。
本研究建立了一种快速、简单、准确的方法,用于测定当归中阿魏酸、松柏醛、藁本内酯的成分。
采用二甲亚砜-d6(DMSO-d6)为测试溶剂,吡嗪为内标物质,在 600 MHz 超导核磁共振波谱仪上进行 1H-qNMR 测量。吡嗪、阿魏酸、藁本内酯和松柏醛的定量共振峰分别位于 δ8.66 ppm、δ6.35-6.37 ppm、δ5.53-5.55 ppm 和 δ6.50-6.53 ppm。
验证了线性关系、检测限、定量限、精密度、稳定性和回收率,结果良好。另一方面,通过高效液相色谱法进行了验证,验证用高效液相色谱法通过了线性、精密度、重复性、稳定性和回收率的方法学考察,结果良好。此外,1H-qNMR 法和 HPLC-UV 法在测定三批当归中三种成分的含量时,结果无显著差异。
该方法可用于同时测定三种活性成分,为当归的整体质量评价和质量控制提供了科学依据。
本研究首次采用 1H-qNMR 测定当归中的阿魏酸、松柏醛和藁本内酯。