定量核磁共振氢谱法测定药用辅料二油酰基磷脂酰胆碱的含量  

Quantitative Analysis of 1,2-Dioleoyl-sn-glycero-3-Phosphocholine in Pharmaceutical Excipients by Proton Nuclear Magnetic Resonance

作　　者：王娅雯 陈雪帆 WANG Yawen;CHEN Xuefan(Green Pharmaceutical Collaborative Innovation Center,Zhejiang University of Technology,Hangzhou 310014,China)

机构地区：[1]浙江工业大学绿色制药协同创新中心,杭州310014

出　　处：《中国药学杂志》2025年第2期184-188,共5页Chinese Pharmaceutical Journal

基　　金：国家药典委员会药品标准制修订研究课题资助(2023Y002)。

摘　　要：目的 建立测定二油酰基磷脂酰胆碱(1,2-dioleoyl-SN-glycero-3-phosphocholine, DOPC)含量的定量核磁共振氢谱法(quantitative proton nuclear magnetic resonance, qHNMR)。方法 采用Bruker AVANCEⅡ600 MHz核磁共振波谱仪,采集DOPC的核磁共振氢谱,以1,3,5-三甲氧基苯为内标物,氘代氯仿为溶剂,30°脉冲,扫描次数为16次,测试温度25℃,采集时间(AQ)为5 s,弛豫延迟时间(D1)为35 s,对DOPC进行定量分析。结果 样品的1H-NMR谱在化学位移δ 0.87出现甲基的质子信号,DOPC和内标物定量峰信号在1H-NMR谱上分离度良好,DOPC在线性范围内线性关系良好(r>0.999 6),方法精密度和重复性良好,DOPC含量为96.7%~98.7%,测定结果与磷钼酸比色法测定结果基本一致。结论 建立的qHNMR方法可以对DOPC进行准确定量,相比于经典的磷钼酸比色方法更加快速,并且不需要复杂的前处理操作。OBJECTIVE To develop a quantitative proton nuclear magnetic resonance(qHNMR)method for the determination of 1,2-dioleoyl-sn-glycero-3-phosphocholine(DOPC).METHODS A Bruker AVANCEⅡ600 MHz NMR resonance spectra was utilized to acquire the NMR spectra of DOPC.The compound 1,3,5-trimethoxybenzene served as the internal standard,deuterated chloroform as the solvent,with 30°pulses,16 scans,a test temperature of 25℃,and an acquisition time(AQ)of 5 s.The relaxation delay time(D1)was set at 35 s for quantitative analysis of DOPC.RESULTS The sample's 1H-NMR spectra displayed a methyl proton signal at chemical shiftδ0.87;the quantitative peak signals of DOPC and internal standard were well resolved on the 1H-NMR spectra with good linear relationship for DOPC(r>0.9996).The method demonstrated accuracy and repeatability with DOPC content ranging from 96.7%to 98.7%,consistent with results obtained from phosphomolybdic acid colorimetry.CONCLUSION The established qHNMR method accurately quantifies DOPC,is faster than the classical phosphomolybdate colometry method,requires no complex pretreatment operations.

关 键 词：定量核磁共振氢谱法 药用辅料 含量测定 内标法 二油酰基磷脂酰胆碱 

分 类 号：R917[医药卫生—药物分析学]