新型^(19)F核磁共振定量技术测定氟哌利多含量

Application of novel ^(19)F quantitative NMR(^(19)F-qNMR)in assay of droperidol

目的:建立用19F核磁共振定量技术测定氟哌利多含量的方法。方法:以4-溴-2-氟乙酰苯胺为内标,CDCl3为溶剂测定19F核磁共振谱,通过比较氟哌利多样品定量峰与内标物质响应峰面积,计算氟哌利多的含量。结果:同一样品在相同条件下测定6次,定量峰与内标响应峰比值的RSD为1.04%;将图谱重复积分5次,定量峰与内标峰比值的RSD为1.01%;平行配制3份样品,依据定量峰与内标响应峰比值计算的氟哌利多平均含量为95.7%,RSD为0.53%,19F核磁共振定量结果与质量平衡法测定结果 95.2%一致。结论:19F核磁共振定量法内标选择广泛,图谱解析简单,可以准确快速测定氟哌利多含量。

Objective：To establish a ^19F-qNMR method to determine the content of droperidol. Methods： 4＇-bromo-2＇-fluoroaeetanilide was used as internal standard, and CDCl3 was used as solvent. The content of droperidol was calculated by comparing the response peak areas of sample （As）and internal standard （Ar）. Results：The RSD of As/Ar of repeated determination of the sample solution was 1.04% （n = 6） ; the RSD of As/Ar of repeated integration of the same spectrum was 1.01% （n = 5 ） ;the mean content of three droperidol samples was 95.7% （RSD 0.53% ）, which was consistent with the result from mass balance method （95.2%）. Conclusion： ^19F-qN- MR can be used to determine the content of droperidol precisely and rapidly.