摘要
建立基于定量核磁共振氢谱(quantitative proton nuclear magnetic resonance,qHNMR)的神曲中葡萄糖含量的测定方法,对市售神曲中葡萄糖的含量进行分析,并探究神曲加工炮制过程中葡萄糖含量的变化规律。以重水为溶剂,2,2,2,3-d4-3-(三甲基硅基)丙酸钠盐为内标,以化学位移δ4.65、5.24处葡萄糖端基质子双峰信号作为定量峰,对神曲中葡萄糖含量进行定量。经方法学评价,葡萄糖在0.10~6.44 mg·mL-1呈现良好的线性关系,精密度、稳定性、重复性和加样回收率试验的RSD均小于2.3%。市售神曲中葡萄糖含量波动明显,推测与神曲的发酵天数、麸面比及炮制方式等有关。神曲中葡萄糖含量随发酵天数增加呈先增加后降低的趋势;全麦麸或全面粉发酵的神曲中葡萄糖含量明显低于麦麸和面粉混合发酵的神曲;麸炒神曲较生神曲葡萄糖含量略有降低,而焦神曲中葡萄糖含量显著降低。该实验建立的qHNMR方法简单快捷,准确度高,为神曲中葡萄糖含量测定提供了新的方法。此外,该研究阐明了神曲加工炮制过程中葡萄糖的量变规律,对判断神曲发酵程度具有指示意义,为揭示神曲的发酵机制,完善神曲的质量控制方法提供了科学依据。
A quantitative proton nuclear magnetic resonance(qHNMR)method was established to determine the glucose content in commercially available Massa Medicata Fermentata(MMF)products and explore the variations of glucose content in MMF products during processing.The qHNMR spectrum of MMF in deuterium oxide was obtained with 2,2,3,3-d4-3-(trimethylsilyl)propionate sodium salt as the internal standard substance.With the doublet peaks of terminal hydrogen of glucose with chemical shift atδ4.65 andδ5.24 as quantitative peaks,the content of glucose in MMF samples was determined.The glucose content showed a good linear relationship within the range of 0.10-6.44 mg·mL-1.The relative standard deviations(RSDs)of precision,stability,repeatability,and recovery for determination were all less than 2.3%.The glucose content varied in different commercially available MMF samples,which were associated with the different fermentation days,wheat bran-to-flour ratios,and processing methods.The glucose content in MMF first increased and then decreased over the fermentation time.Compared with the MMF products fermented with wheat bran or flour alone,the products fermented with both wheat bran and flour had increased glucose.The glucose content of bran-fried MMF was slightly lower than that of raw MMF,while the glucose content in charred MMF was extremely low.In conclusion,the qHNMR method established in this study is simple,fast,and accurate,serving as a new method for determining the glucose content in MMF.Furthermore,this study clarifies the variations of glucose content in MMF during processing,which can not only indicate the processing degree but also provide a scientific basis for revealing the fermentation mechanism and improving the quality control of MMF.
作者
石亚玲
单鲁豫
杨晶晶
姜苗苗
于卉娟
王跃飞
柴欣
SHI Ya-ling;SHAN Lu-yu;YANG Jing-jing;JIANG Miao-miao;YU Hui-juan;WANG Yue-fei;CHAI Xin(National Key Laboratory of Chinese Medicine Modernization,Tianjin Key Laboratory of TCM Chemistry and Analysis,Institute of Traditional Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;Haihe Laboratory of Modern Chinese Medicine,Tianjin 301617,China)
出处
《中国中药杂志》
CSCD
北大核心
2023年第23期6396-6402,共7页
China Journal of Chinese Materia Medica
基金
国家重点研发计划项目(2021YFC1712905)
现代中医药海河实验室科技项目(22HHZYSS00007)
山东省自然科学基金创新发展联合基金项目(ZR2021LZY035)。
关键词
定量核磁共振氢谱法
神曲
葡萄糖
发酵天数
麸面比
炮制
quantitative proton nuclear magnetic resonance
Massa Medicata Fermentata
glucose
fermentation days
wheat branto-flour ratio
processing
