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快速扫描四极杆质谱仪在水中农药的全二维气相色谱分析中的性能评估。

Performance evaluation of a rapid-scanning quadrupole mass spectrometer in the comprehensive two-dimensional gas chromatography analysis of pesticides in water.

机构信息

Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università degli Studi di Messina, Messina, Italy.

出版信息

J Sep Sci. 2011 Sep;34(18):2411-7. doi: 10.1002/jssc.201100085. Epub 2011 Jul 28.

DOI:10.1002/jssc.201100085
PMID:21796783
Abstract

The performance of a novel rapid-scanning (20,000 amu/s) quadrupole mass spectrometer (qMS) has been evaluated in the comprehensive 2-D gas chromatography (GC×GC) analysis of pesticides contained in water. Analyte extraction was performed by using direct solid-phase microextraction (SPME). The MS system was operated using a rather wide m/z 50-450 mass range and a 33 Hz spectral production rate, a frequency which was found sufficient for reliable quantification. The qMS performance was evaluated considering: (i) number of data points per peak, (ii) mass spectral quality, (iii) extent of peak skewing, and (iv) consistency of retention times. Seven-point calibration curves (external calibration) were constructed for 28 pesticides over the limit of quantification range of 100 μg/L (1, 5, 10, 25, 50, and 100 μg/L). The solid-phase microextraction-GC×GC-qMS method was validated by calculating limits of detection and quantification, intraday peak area precision, accuracy, and intraday retention-time precision. A series of tap water samples were subjected to analysis, fortunately giving negative results.

摘要

新型快速扫描(20,000 amu/s)四极杆质谱仪(qMS)的性能在水中农药的全二维气相色谱(GC×GC)分析中进行了评估。采用直接固相微萃取(SPME)进行分析物提取。MS 系统的操作使用相当宽的 m/z 50-450 质量范围和 33 Hz 的光谱产生速率,发现该频率足以进行可靠的定量。考虑了 qMS 的性能:(i)每个峰的数据点数量,(ii)质谱质量,(iii)峰倾斜程度,和(iv)保留时间的一致性。对于 28 种农药,在 100 μg/L(1、5、10、25、50 和 100 μg/L)的定量限范围内,建立了七点校准曲线(外部校准)。通过计算检测限和定量限、日内峰面积精密度、准确度和日内保留时间精密度对固相微萃取-GC×GC-qMS 方法进行了验证。对一系列自来水样品进行了分析,幸运的是得到了阴性结果。

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