邻苯二甲酸酯类标准物质核磁共振定量方法的建立  

Establishment of a quantitative 1H-NMR method for phthalate esters standard material analysis

作　　者：张琪[1] 朱红波 吴先富[1] 杨化新[1] 马玲云[1] 李晓东[1] 肖新月[1] 

机构地区：[1]中国食品药品检定研究院,北京100050 [2]西藏自治区食品药品检验所,拉萨850000

出　　处：《药物分析杂志》2015年第7期1287-1291,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：重大新药创制课题-化学新药质量标准研究与评价技术平台(项目编号:2011ZX09303-001)

摘　　要：目的:建立以核磁共振定量法(简称qNMR法)测定邻苯二甲酸酯标准物质含量。方法:仪器为配备5 mm BBO探头的Bruker Ascend 500 MHz核磁共振仪,采集一维定量氢谱,90°脉冲,延迟时间的d1为20 s,温度为25℃,采样次数为128次。以富马酸为内标,对12种邻苯二甲酸酯类标准物质进行定量研究。结果:12种邻苯二甲酸酯标准物质qNMR法测定结果与对照品标定的质量平衡法定值结果基本一致。结论:采用qNMR法研究建立邻苯二甲酸酯标准物质含量测定方法,方法快捷、准确,是对标准物质量值定量测定的一种良好的补充。Objective ： To develop a nuclear magnetic resonance （qNMR） method for the quantitative determination of phthalate esters standard materials. Methods：1H-NMR spectra were collected at Bruker Ascend 500 spectrome- ter with 5 mm BBO probe. The internal standard was fumaric acid. The parameter setup was as follows： 90° pulse sequences, dl was 20 s,temperature was 25 ℃, and the number of scan was 128. Results ：The qNMR results of 12 phthalate esters standard materials were consistent with the results obtained from mass balance methods. Conclusion：qNMR method is a good supplementary quantitative method for standard materials, which can be used for the rapid quantitative determination of phthalate esters standard materials.

关 键 词：核磁共振定量 邻苯二甲酸酯类 标准物质定量分析 富马酸内标物 

分 类 号：R917[医药卫生—药物分析学]