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[摘要]
目的 建立核磁共振法测定13-顺阿维A。方法 采用1H-NMR测定13-顺阿维A,通过样品与内标物质响应峰面积比较计算样品的质量分数以及其中残留溶剂。结果 以δ5.64处定量峰和δ8.45处内标峰面积比值与13-顺阿维A和1,4-对硝基苯质量比进行线性回归,线性关系良好。13-顺阿维A的质量分数为98.5%,RSD值为1.5%(n=3),重复性良好,与质量平衡法测定结果一致;样品中残留溶剂为四氢呋喃,其质量分数为1.0%。结论 核磁共振法测定13-顺阿维A快速、准确、方便,结果可靠,可以用来进行标准物质的测定。
[Key word]
[Abstract]
Objective To establish a nuclear magnetic resonance (NMR) method to determine the content of 13-cis acitretin. Methods 1H-NMR was used to characterize 13-cis acitretin. The mass fraction and residue solvent of 13-cis acitretin were calculated by comparing the peak area of 13-cis acitretin with the internal reference substance. Results There was a good regression between quantitative peaks ration of 13-cis acitretin and internal reference substance versus mass ratio of δ5.64 and 8.45. Based on NMR, the mass fraction of 13-cis acitretin was 98.5% with RSD of 1.5% (n = 3) and the residual solvent was tetrahydrofuran with its mass fraction of 1.0%. Conclusion It is a rapid, convenient, and precise method for the determination of 13-cis acitretin by NMR, and the results can be used in reference substance assay experiment.
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[基金项目]
国家重大新药创制专项(2011ZX09303-001);国家质量监督检验检疫总局公益性行业科研专项(2012104008-1-14)