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同时微萃取和衍生化后 GC-MS 快速分析醛类。

Rapid analysis of aldehydes by simultaneous microextraction and derivatization followed by GC-MS.

机构信息

Key Laboratory of Applied Organic Chemistry, Higher Institutions of Jiangxi Province, Shangrao Normal University, Shangrao, PR China.

出版信息

J Sep Sci. 2011 Jul;34(13):1607-12. doi: 10.1002/jssc.201100145. Epub 2011 May 19.

Abstract

Ultrasound-assisted dispersive liquid-liquid microextraction (UDLLME) and simultaneous derivatization followed by GC-MS was developed for the analysis of four aldehydes including acetaldehyde (ACE), propionaldehyde (PRO), butyraldehyde (BUT) and valeraldehyde (VAL) in water samples. In the proposed method, the aldehydes were derivatized with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine (PFBHA) and extracted by UDLLME in aqueous solution simultaneously; finally, the derivatives were analyzed by GC-MS. The experimental parameters were investigated and the method validations were studied. The optimal conditions were: aqueous sample of 5 mL, PFBHA of 50 μL, 1.0 mL ethanol (disperser solvent) containing 20 μL chlorobenzene (extraction solvent), ultrasound time of 2 min and centrifuging time of 3 min at 6000 rpm. The proposed method provided satisfactory precision (RSD 1.8-10.2%), wide linear range (0.8-160 μg/L), good linearity (R(2) 0.9983-0.9993), good relative recovery (85-105%) and low limit of detection (0.16-0.23 μg/L). The proposed method was successfully applied for the analysis of aldehydes in water samples. The experimental results showed that the proposed method was a very simple, rapid, low-cost, sensitive and efficient analytical method for the determination of trace amount of aldehydes in water samples.

摘要

超声辅助分散液液微萃取(UDLLME)和同时衍生化后 GC-MS 用于分析水样中的四种醛,包括乙醛(ACE)、丙醛(PRO)、丁醛(BUT)和戊醛(VAL)。在该方法中,醛与 O-2,3,4,5,6-(五氟苄基)羟胺(PFBHA)衍生化,并在水溶液中通过 UDLLME 同时萃取;最后,通过 GC-MS 分析衍生物。研究了实验参数并进行了方法验证。最佳条件为:5 mL 水样、50 μL PFBHA、1.0 mL 含 20 μL 氯苯(萃取溶剂)的乙醇(分散溶剂)、超声时间 2 min 和 6000 rpm 下离心时间 3 min。该方法提供了令人满意的精密度(RSD 1.8-10.2%)、宽线性范围(0.8-160 μg/L)、良好的线性(R² 0.9983-0.9993)、良好的相对回收率(85-105%)和低检测限(0.16-0.23 μg/L)。该方法成功应用于水样中醛的分析。实验结果表明,该方法是一种非常简单、快速、低成本、灵敏和高效的分析方法,用于测定水样中痕量醛。

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