基于磁化阴离子交换型金属有机骨架材料的磁固相萃取-离子色谱法测定沙坦类药物中的叠氮化物
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摘要
叠氮化物是沙坦类药物必不可少的原料之一,最终产品中易引入叠氮根离子,但因为叠氮化物是剧毒物质,容易对人体造成伤害。本文采用磁化季胺型阴离子交换金属有机骨架(MOFs)MIL-101(Cr)-NMe_3作为磁固相萃取剂,对沙坦类药物中残余的叠氮根离子进行富集萃取。考察了分离萃取条件,包括pH、萃取剂用量、萃取时间、解吸剂种类及用量,得出最佳萃取条件。再使用离子色谱(IC)法测定叠氮根离子含量。详细考察了色谱条件,包括分析柱的选择、流动相的组成和浓度、柱温、流速等,得出最佳色谱检测条件。方法重复性良好,回收率在93.8%~98.5%之间,最低检测限为0.23μg·L~(-1),检测的线性范围在0.01~1mg·L~(-1),其相关系数r~2为0.9998。实验结果表明:采用该方法可以将药物中的各类杂质与待测组分有效分离,简化样品预处理过程,提高测定灵敏度,降低检测成本。
Azide is a kind of indispensable raw material of sartan,and it may exists in the final products.However,azide is similar to cyanide,belongs to the highly toxic substances,which can damage to human health.In this paper,we integration of anionic-exchange metal-organic frameworks(MOFs) MIL-101(Cr)-NMe_3 with magnets for magnetic solid-phase extraction for separation and enrichment of azide ion in sartan.Then the azide is determined by ion chromatography(IC).The conditions of extraction and IC were examined in detail.The method is simple,accurate and rapid,the recovery is in the 93.8%~98.5%,detection line is 0.23 μg·L~(-1),linearity range is 0.01~1 mg·L~(-1) and linearly dependent coefficient(r~2) is 0.9998.
引文
[1]Huo,S H.;Yan,X P.Analyst.2012,137:3445-3451.
    [2]Liu,K;Zhang,S Y;Hu,X Y;Zhang K Y;Roy,A;Yu,G.Environ.Sci.Technol.2015,49:8657-8665.
    [3]黄巧巧,何佳佳,钟乃飞,郑国刚.药物分析杂志,2013,33(8):1431-1434.

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