摘要
目的:建立间接定量核磁共振氢谱(^(1)H qNMR)法测定山梨酸钾的含量,以期应用于其他同类型的药用辅料及化合物的含量测定。方法:以DMSO为参比物并溶于重水形成参比溶液,将适量的待测物(山梨酸钾)和标准物质(马来酸)分别与等体积的参比溶液混合制样并分别测定核磁氢谱,在对待测物、标准物质和参比物的核磁定量峰积分的基础上,以参比物的峰面积为基准,建立待测物的定量计算公式,并对多批样品的含量进行测试和计算。结果:方法学研究表明,该方法具有良好的线性关系(r=0.9998),线性范围以比值K[(山梨酸钾/参比物DMSO定量特征峰面积比)/(马来酸/参比物DMSO定量特征峰面积比)]为参考,其范围约为0.18~3.07,精密度试验RSD为0.13%,重复性试验RSD为0.38%,与2020年版《中华人民共和国药典》记载的山梨酸钾含量测定方法进行对照,两种方法对多批样品的定量结果基本一致。结论:建立的^(1)H qNMR法操作简便,样品用量少,结果较准确,适用于内标和样品不相容的情况及其他的应用场景。
Objective:To establish a quantitative nuclear magnetic resonance hydrogen spectroscopy(^(1)H qNMR)method for indirectly determining the content of potassium sorbate,in order to apply it to the determination of the content of other similar pharmaceutical excipients and compounds.Method:DMSO was used as a reference substance and dissolved in heavy water to form a reference solution.An appropriate amount of the test substance(potassium sorbate)and the standard substance(maleic acid)were mixed with equal volumes of the reference solution to prepare samples,and the ^(1)H qNMR were measured respectively.Based on the integration of the nuclear magnetic quantification peaks of the test substance,the standard substance,and the reference substance,a quantitative calculation formula for the test substance was established using the peak area of the reference substance as the reference,and the content of multiple batches of samples was tested and calculated.Result:Methodological studies showed that this method had a good linear relationship(r=0.9998).The linear range was based on the ratio K[(potassium sorbate/reference DMSO quantitative characteristic peak area ratio)/(maleic acid/reference DMSO quantitative characteristic peak area ratio)],which was approximately 0.18-3.07.The precision RSD was 0.13%,and the repeatability RSD was 0.38%.Compared with the potassium sorbate content determination method recorded in the Chinese Pharmacopoeia(2020),the quantitative results of the two methods for multiple batches of samples were basically consistent.Conclusion:The established ^(1)H qNMR method is easy to operate,requires a small amount of sample,and yields accurate results.It is suitable for situations where internal standards and samples are incompatible,as well as other application scenarios.
作者
陈新启
温静
张家懿
张梅
焦晓林
王尉
CHEN Xin-qi;WEN Jing;ZHANG Jia-yi;ZHANG Mei;JIAO Xiao-lin;WANG Wei(Institute of Analysis and Testing,Beijing Academy of Science and Technology(Beijing Center for Physical and Chemical Analysis),Beijing 100089,China;Biomedicine School,Beijing City University,Beijing 100094,China)
出处
《药物分析杂志》
北大核心
2025年第9期1504-1510,共7页
Chinese Journal of Pharmaceutical Analysis
关键词
定量核磁共振氢谱
药品
辅料
山梨酸钾
含量测定
马来酸
^(1)H qNMR
medicine
excipients
potassium sorbate
content determination
maleic acid
