氢定量核磁共振法测定金丝桃苷标准物质纯度  

Purity Assignment of Hyperoside CRMs by^1H-qNMR

作　　者：王萌玉 全灿[2] 孙永跃[1] 李蔚 WANG Meng-yu;QUAN Can;SUN Yong-yue;LI Wei(Tianjin Key Laboratory of Drug Targeting and Bioimaging,School of Chemistry and Chemical Engineering,Tianjin University of Technology,Tianjin 300384,China;Division of Metrology in Chemistry,National Institute of Metrology,Beijing 100029,China)

机构地区：[1]天津理工大学化学化工学院天津市药物靶向与生物成像重点实验室,天津300384 [2]中国计量科学研究院化学计量与分析科学研究所,北京100029

出　　处：《化学试剂》2020年第4期425-429,共5页Chemical Reagents

摘　　要：基于核磁谱峰的积分信号与产生此信号的原子核数成正比的原理,建立准确的氢定量核磁共振法(1H-qNMR)测定金丝桃苷标准物质(CRMs)纯度,并评估不确定度。实验以二甲基亚砜(DMSO-d6)为氘代溶剂,尼泊金乙酯GBW(E)100064为内标物,谱宽为16 ppm,激发偏置为5.23 ppm,弛豫延迟时间为12 s,扫描次数为32次,采用金丝桃苷化学位移(δ6.21)为定量峰,尼泊金乙酯化学位移(δ4.24)为内标峰,定量金丝桃苷纯度。1H-qNMR测得金丝桃苷纯度为91.86%,精密度RSD为0.085%,重复性RSD为0.53%,质量浓度在9.85~32.02 g/L范围内的线性关系为:y=6.3355x-0.1556(R^2=0.9988,y、x分别代表金丝桃苷与尼泊金乙酯的质量比和积分信号比),评估不确定度为0.55%。1H-qNMR测定结果与质量平衡法一致,表明氢定量核磁共振法适用于金丝桃苷的定量分析。Based on the principle that the integrated signal of NMR peak is proportional to the number of nucleus producing this signal,an accurate hydrogen quantitative nuclear magnetic resonance(1H-qNMR)method is established to determine the purity assignment of hyperoside CRMs and evaluate the uncertainty.The experiment used dimethyl sulfoxide(DMSO-d6)as the deuteration reagent,and ethylparaben was used as the internal standard.The spectral width(SW)was 16 ppm,and the excitation bias(OIP)was 5.23 ppm,relaxation delay time(DI)is 12 s,number of scans(NS)is 32.The chemical shift(δ6.21)of hyperoside was used as the quantitative peak,and the chemical shift(δ4.24)of ethylparaben was used as the internal standard peak to quantify the purity of hyperoside.The purity of hyperoside was 91.86%as determined by 1H-qNMR,the precision RSD was 0.085%,the repetitive RSD was 0.53%.The linear regression equation with mass concentration in the range of 9.85~32.02 g/L is:y=6.3355x-0.1556(correlation coefficient R^2=0.9988,y and x represent the mass ratio and integral area ratio of hyperoside and ethyl p-hydrobenzoate respectively),and the uncertainty of the qNMR measurement result was 0.55%.The purity of the hyperoside measured by 1H-qNMR was consistent with the results of the mass balance method,indicating that the hydrogen quantitative nuclear magnetic resonance method is suitable for the quantitative analysis of hyperoside.

关 键 词：金丝桃苷 氢定量核磁共振法(~1H-qNMR) 定量分析 质量平衡法 不确定度 标准物质 

分 类 号：O657.61[理学—分析化学]