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基于分子印迹聚合物选择性分离后,采用负离子电喷雾离子淌度谱法测定人尿液和血浆中的水杨酸。

A new approach to determine salicylic acid in human urine and blood plasma based on negative electrospray ion mobility spectrometry after selective separation using a molecular imprinted polymer.

机构信息

Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.

出版信息

Talanta. 2012 Sep 15;99:520-6. doi: 10.1016/j.talanta.2012.06.023. Epub 2012 Jun 19.

Abstract

This paper deals with a method based on negative electrospray ionization ion mobility spectrometry (ESI-IMS) as a detection technique. The method was used to determine the salicylic acid in human urine and plasma after selective separation of salicylic acid (SA) via molecular imprinted polymer (MIP). The ion mobility spectrum of salicylic acid in negative mode and the reduced mobility value for its ion peak is reported in this paper for the first time. In order to combine the technique with negative ESI-IMS, suitable experimental conditions related to MIP (e.g., Soxhlet extraction) were selected. The method was exhaustively validated in terms of sensitivity, imprinting factor, enrichment factor, and sorption capacity. The linear dynamic range of 0.02-2.00 μg mL(-1) and the relative standard deviation (RSD) below 6% were obtained for the analysis of SA through this method. The average recovery was calculated about 92% for the analyzed drug. Finally, human urine and plasma were analyzed and the feasibility of the proposed method was successfully verified by the efficient clean-up of the samples using MIP separation before the analysis by ESI-IMS.

摘要

本文研究了一种基于负电喷雾电离离子淌度谱(ESI-IMS)的方法作为检测技术。该方法用于通过分子印迹聚合物(MIP)选择性分离水杨酸(SA)后,测定人尿液和血浆中的水杨酸。本文首次报道了负模式下水杨酸的离子淌度谱及其离子峰的还原淌度值。为了将该技术与负 ESI-IMS 相结合,选择了与 MIP 相关的合适实验条件(例如索氏提取)。该方法在灵敏度、印迹因子、富集因子和吸附容量方面进行了全面验证。通过该方法分析 SA 的线性动态范围为 0.02-2.00μgmL(-1),相对标准偏差(RSD)低于 6%。分析药物的平均回收率约为 92%。最后,分析了人尿液和血浆,并通过 MIP 分离在 ESI-IMS 分析前对样品进行有效的净化,成功验证了该方法的可行性。

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