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固相微萃取-气相色谱-质谱法同时测定水样中紫外滤光剂和多环麝香

Simultaneous determination of UV filters and polycyclic musks in aqueous samples by solid-phase microextraction and gas chromatography-mass spectrometry.

机构信息

Hygiene Detection Center, School of Public Health and Tropical Medicine, Southern Medical University, Guangzhou 510515, China.

出版信息

J Chromatogr A. 2010 Oct 22;1217(43):6747-53. doi: 10.1016/j.chroma.2010.06.004. Epub 2010 Jun 9.

Abstract

A simple, precise and accurate method for the simultaneous determination of four UV filters and five polycyclic musks (PCMs) in aqueous samples was developed by solid-phase microextraction coupled with gas chromatography-mass spectrometry (SPME-GC-MS). The operating conditions affecting the performance of SPME-GC-MS, including fiber thickness, desorption time, pH, salinity, extraction time and temperature have been carefully studied. Under optimum conditions (30 μm PDMS fiber, 7 min desorption time, pH 7, 10% NaCl, 90 min extraction time at 24°C), the correlation coefficients (r(2)) of the calibration curves of target compounds ranged from 0.9993 to 0.9999. The limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.2 to 9.6 ng L⁻¹ and 0.7 to 32.0 ng L⁻¹, respectively. The developed procedure was applied to the determinations of four UV filters and five PCMs in river water samples and internal standard was used for calibration to compensate the matrix effect. Good relative recoveries were obtained for spiked river water at low, medium and high levels. The proposed SPME method was compared with traditional SPE procedure and the results found in river water using both methods were in the same order of magnitude and both are quite agreeable.

摘要

建立了固相微萃取结合气相色谱-质谱法(SPME-GC-MS)同时测定水样中四种紫外滤光剂和五种多环麝香的简单、准确、精确的方法。详细研究了影响 SPME-GC-MS 性能的操作条件,包括纤维厚度、解吸时间、pH 值、盐度、萃取时间和温度。在最佳条件下(30μmPDMS 纤维,7min 解吸时间,pH7,10%NaCl,24°C 下萃取 90min),目标化合物校准曲线的相关系数(r²)范围为 0.9993 至 0.9999。检测限(LOD)和定量限(LOQ)范围分别为 0.2 至 9.6ngL⁻¹和 0.7 至 32.0ngL⁻¹。所开发的程序用于测定河水中的四种紫外滤光剂和五种多环麝香,并使用内标进行校准以补偿基质效应。在低、中、高浓度下,对河水进行加标回收,得到了良好的相对回收率。将所提出的 SPME 方法与传统 SPE 程序进行了比较,两种方法在河水中的结果均处于同一数量级,且均非常吻合。

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