去卷积定量核磁共振法测定缩宫素纯度  

Measurement of the Purity of Oxytocin by Quantitative Nuclear Magnetic Resonance Method with Deconvolution

作　　者：黄挺[1] 张伟[1] 李红梅[1] HUANG Ting;ZHANG Wei;LI Hong-mei(Chemical Metrology&Analytical Science Division,National Institute of Metrology,Beijing 100029,China)

机构地区：[1]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：《计量学报》2023年第8期1298-1302,共5页Acta Metrologica Sinica

基　　金：中国计量科学研究院项目(21-AKYZZ2120-21)。

摘　　要：缩宫素是重要的肽,被选择为相对分子量5000以下、交联且无修饰的肽类的代表,作为纯度计量国际比对的分析目标物。建立了一种去卷积定量核磁共振法,用于测定含有大量结构类似杂质的缩宫素样品的纯度,选择合适的内标(安赛蜜)、溶剂(重水)、定量峰(化学位移=7.1的苯基氢)以及实验参数,通过去卷积分析,获得与定量峰重叠的3个杂质峰的面积,扣减了杂质峰的面积,准确测定了缩宫素的纯度。使用所述方法参加了国际比对,结果(785.8 mg/g,扩展不确定度15.4 mg/g)与比对参考值(787.2 mg/g,扩展不确定度12.9 mg/g)一致;而且,与其它常用方法相比,所述方法的操作简便,分析时间短,成本低。结果表明该方法是一种准确、快速、简便的肽纯度定值方法。Oxytocin is an important peptide,and it was chosen as the target analyte of the purity metrological international comparison,representing the type of peptide with molecular weight<5000,cross-linking,and non-modification.A quantitative nuclear magnetic resonance method with deconvolution was established to measure the purity of the oxytocin sample containing many structurally similar impurities.Appropriate internal standard(acesulfame potassium),solvent(deuterium oxide),quantitative peak(phenyl protons at chemical shift=7.1)and experimental parameters were selected.Through deconvolution analysis,the areas of three impurity peaks overlapping with the quantitative peak were obtained.After deducting the areas of impurity peaks,the purity of the oxytocin sample was accurately determined.The mentioned method was applied to participate in that international comparison,and its result(785.8 mg/g,with expanded uncertainty of 15.4 mg/g)was consistent with the reference value of the comparison(787.2 mg/g,with expanded uncertainty of 12.9 mg/g).Moreover,compared with other common methods,the method has the advantages of simple operation,short analysis time and low cost.The results show that the mentioned method is an accurate,rapid and simple method for peptide purity determination.

关 键 词：计量学 缩宫素 纯度测定 去卷积 定量核磁共振 肽 

分 类 号：TB99[一般工业技术—计量学]