Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università degli Studi di Messina, Messina, Italy.
J Sep Sci. 2011 Sep;34(18):2411-7. doi: 10.1002/jssc.201100085. Epub 2011 Jul 28.
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.
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。