反门控去耦技术-定量核磁共振法测定染料木素的含量  

Determination of Genistein by Quantitative Nuclear Magnetic Resonance with Inverse Gated Decoupling Technology

作　　者：李永利[1] 陈鹰[1] 李杰[1] LI Yongli;CHEN Ying;LI Jie(Shanghai Key Laboratory of Online Testing and Control Technology,Physical and Chemical Analysis Laboratory,Shanghai Institute of Measurement and Testing Technology,Shanghai 201203,China)

机构地区：[1]上海市计量测试技术研究院理化分析室,上海市在线检测与控制技术重点实验室,上海201203

出　　处：《理化检验（化学分册）》2022年第6期629-633,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海市计量测试技术研究院项目(I00RY1911)。

摘　　要：以香草扁桃酸为内标物,提出了测定染料木素的定量核磁共振法(qNMR).采用反门控去耦模式采集氢谱,驰豫延迟时间为40 s,扫描次数为32次,采集时间为4.0 s,溶剂为氘代二甲亚砜,以染料木素中化学位移(δ,×10^(-6))6.38的峰为定量峰,香草扁桃酸中δ6.96为内标物信号峰.结果表明,染料木素与内标物香草扁桃酸的质量比在0.83~7.50内,与其定量峰和内标物信号峰的峰面积比值呈线性关系,检出限(3.3s/k)为0.2 g􀅰L^(-1).在精密度试验中,测定值的相对标准偏差(n=6)均小于0.35%;稳定性试验显示供试品溶液在避光条件下24 h内稳定.方法用于实际样品的分析,测定结果与国家标准GB/T 23788-2009的一致.A method for determination of genistein by quantitative nuclear magnetic resonance(qNMR)was proposed,using vanilmandelic acid as the internal standard.The measurement conditions with inverse gated decoupling technology were as follows:the relaxation delay time was 40 s,the number for scanning was 32,the acquisition time was 4.0 s,and the solvent was deuterated dimethyl sulfoxide.The peak ofδ6.38 in genistein was selected as the quantitative peak,and peak ofδ6.96 in vanilmandelic acid was selected as the internal standard signal peak.As shown by the results,linear relationship between the peak area ratio of quantitative peak to internal standard signal peak and mass ratio of genistein to vanillic acid was found in the range of 0.83-7.50,with detection limit(3.3s/k)of 0.2 g·L^(-1).And RSDs of the determined values(n=6)was less than 0.35%in the precision test.The stability test showed that the test solution was stable for 24 h in the dark.This method was applied to the analysis of actual samples,and the determination result was consistent with that of the national standard GB/T 23788-2009.

关 键 词：染料木素 定量核磁共振法 反门控去耦技术 

分 类 号：O657.61[理学—分析化学]