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

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.

The penetration of green sample-preparation techniques in comprehensive two-dimensional gas chromatography

“…TIC SPME-GC×GC-qMS chromatogram of a pesticide mixture in drinking water at the 10-ppb level. For peak identification refer to [27]. (Reproduced with permission from Wiley).…”

“…Purcaro et al exploited the enrichment capability of SPME coupled to GC×GC combined with a rapid-scanning qMS instrument for the determination of pesticides in drinking water [27]. A 100-μm PDMS fiber was directly immersed in drinking water to extract pesticides.…”

Cryogenic modulation fast GC × GC–MS using a 10 m microbore column combination: Concept, method optimization, and application

“…GC × GC was first reported in 1991 by Liu and Phillips . This now well‐known multidimensional technology is commonly performed by using a conventional column (i.e., 30 m × 0.25 mm id × 0.25 μm d f ) as first dimension ( 1 D), and a short micro‐bore column segment (i.e., 1–2 m × 0.1 mm id × 0.1 μm d f ) as second dimension ( 2 D) . The analysis timeframes are about the same as those observed in 1D GC applications (1–2 h), even though variations do exist.…”

“…GC × GC was first reported in 1991 by Liu and Phillips [1]. This now well-known multidimensional technology is commonly performed by using a conventional column (i.e., 30 m × 0.25 mm id × 0.25 μm d f ) as first dimension ( 1 D), and a short micro-bore column segment (i.e., 1-2 m × 0.1 mm id × 0.1 μm d f ) as second dimension ( 2 D) [2][3][4]. The analysis timeframes are about the same as those observed in 1D GC applications (1-2 h), even though variations Abbreviations: 1 D, first dimension; 2 D, second dimension; CM, cryogenic modulation; LRI, linear retention index; QMS, quadrupole mass spectrometry; SCCS, Scientific Committee on Consumer Safety Conflict of interest: The authors declare no financial/commercial conflict of interest.…”

Impact of comprehensive two‐dimensional gas chromatography with mass spectrometry on food analysis

“…Even though to a much lower extent, compared to LR‐TOF‐MS, rapid scanning qMS instruments have been used for targeted GC×GC applications on pesticide contaminants. For example, Purcaro et al evaluated the analytical performance of a powerful qMS system (scan speed: 20 000 amu/s) for the determination of pesticides in drinking water . High sensitivity is required in such applications because European regulations limit the presence of pesticides in drinking water at an MRL of 0.1 μg/L.…”