College of Nursing, Hebei University, Baoding, P. R. China.
College of Chemistry and Environmental Science, Hebei University, Baoding, P. R. China.
J Sep Sci. 2022 Jun;45(11):1874-1883. doi: 10.1002/jssc.202200003. Epub 2022 Apr 15.
A novel thiolysis-high-performance liquid chromatography method for the quantitative determination of total proanthocyanidins and the mean degree of polymerization in grape seeds has been developed. Following thiolysis with formic acid and benzyl mercaptan, reaction products were separated and purified. Three proanthocyanidin monomers and three derivatives were obtained and their structures were identified by liquid chromatography-mass spectrometry, FTIR spectroscopy, and NMR spectroscopy. A decomposition model of the thiolysis products and a correction formula for proanthocyanidins concentration were established. This thiolysis-high-performance liquid chromatography method displayed good calibration linearity (R > 0.999 over the concentration range 0.01 to 10 mg/mL), excellent accuracy (recoveries of 97.9-99.6%), and precision (repeatability relative standard deviations of 0.45-0.75%). This method is suitable for the quantitative analysis of proanthocyanidins in grape seed products.
建立了一种新型的巯解-高效液相色谱法，用于定量测定葡萄籽中原花青素总量和平均聚合度。用甲酸和苯硫醇进行巯解后，分离和纯化反应产物。得到三种原花青素单体和三种衍生物，并通过液相色谱-质谱、傅里叶变换红外光谱和核磁共振波谱对其结构进行了鉴定。建立了巯解产物的分解模型和原花青素浓度的校正公式。该巯解-高效液相色谱法具有良好的校准线性（浓度范围为 0.01 至 10mg/mL 时，R>0.999）、出色的准确性（回收率为 97.9-99.6%）和精密度（重复性相对标准偏差为 0.45-0.75%）。该方法适用于葡萄籽油制品中原花青素的定量分析。
