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用于搅拌棒吸附萃取与离子迁移谱联用的进样口的设计与构建。

Design and construction of an injection port for coupling stir-bar sorptive extraction with ion mobility spectrometry.

作者信息

Jafari Mohammad T, Rezayat Mohammad R, Mossaddegh Mehdi

机构信息

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

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

出版信息

Talanta. 2018 Feb 1;178:369-376. doi: 10.1016/j.talanta.2017.09.061. Epub 2017 Sep 22.

Abstract

An appropriate injection port was designed and constructed for direct analysis of stir-bar sorptive extractions using an ion mobility spectrometry (IMS). The novel design of the port offers great simplicity in use, high sensitivity, and high thermal and mechanical stability. The sol-gel technique was applied to prepare polydimethylsiloxane absorbent on a stir-bar. The parameters affecting extraction efficiency including stirring rate, extraction temperature, extraction time, salt addition and desorption temperature were optimized. The detection limit of the method was calculated to be 1.5μgL, for diazinon, an organophosphorus pesticide selected as a test compound. The linear dynamic range was obtained to be 5.0-200.0μgL with a determination coefficient of 0.9991 for the test compound. The intra- and inter-day relative standard deviations were calculated to be 4% and 5%, respectively. Agricultural wastewater, well water, and apple were selected as real samples. The detection limit was calculated to be 1.5μgL and 7.5μgkg for the real water samples and the apple sample, respectively. The recovery values (%) were 105 ± 6, 107 ± 3 and 96 ± 6 for the spiked agricultural wastewater, well water and apple samples, respectively. The results revealed that the injection port can be used for direct analysis of samples extracted by any sorbent support, without any further sample preparation.

摘要

设计并构建了一个合适的进样口,用于使用离子迁移谱(IMS)对搅拌棒吸附萃取物进行直接分析。该进样口的新颖设计使用起来非常简便,具有高灵敏度以及高热稳定性和机械稳定性。采用溶胶 - 凝胶技术在搅拌棒上制备聚二甲基硅氧烷吸附剂。对影响萃取效率的参数,包括搅拌速率、萃取温度、萃取时间、加盐量和解吸温度进行了优化。以有机磷农药二嗪农作为测试化合物,该方法的检测限计算为1.5μg/L。测试化合物的线性动态范围为5.0 - 200.0μg/L,测定系数为0.9991。日内和日间相对标准偏差分别计算为4%和5%。选择农业废水、井水和苹果作为实际样品。实际水样和苹果样品的检测限分别计算为1.5μg/L和7.5μg/kg。加标农业废水、井水和苹果样品的回收率(%)分别为105±6、107±3和96±6。结果表明,该进样口可用于对任何吸附剂载体萃取的样品进行直接分析,无需进一步的样品制备。

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