Large-volume injection in residue analysis with capillary gas chromatography using a conventional autosampler and injection by programmed-temperature vaporization with solvent venting

Stan, Hans‐Jürgen; Linkerhägner, Manfred

doi:10.1016/0021-9673(95)01171-4

Cited by 42 publications

(15 citation statements)

References 23 publications

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“…A retention gap, typically 5 m, is recommended [13], but the configuration of RH-GC does not permit the use of a retention gap. Thus, the initial temperature of the column was optimised by observing the peak height as a function of temperature over the range 50-1008C.…”

Section: Rh-gc Parametersmentioning

confidence: 99%

Application of programmable temperature vaporisation injection with resistive heating‐gas chromatography flame photometric detection for the determination of organophosphorus pesticides

Patel¹,

Fussell²,

Goodall

et al. 2006

J of Separation Science

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The combination of a programmable temperature vaporisation (PTV) injector with resistive heating GC (RH-GC), a form of fast GC, has been applied to the analysis of organophosphorus (OP) pesticides. The PTV injector was optimised in the 'at-once' solvent vent mode for the injection of ethyl acetate (10-40 microL) or ACN (10 microL). The short RH-GC column (5 m x 0.25 mm ID) with fast temperature ramps (up to 153 degrees C/ min) allowed the separation of a total of 20 OP pesticides in less than 6 min. Average recoveries between 67 and 119% were obtained for pesticides spiked at 0.01 mg/kg into apple and pear matrix. Extraction of orange juice with ACN provided higher recoveries (92-104%) for methamidophos, acephate and omethoate compared to ethyl acetate (62-73%). Results for analysis of OP pesticides in samples containing incurred residues were in good agreement with those obtained using GC-MS. The overall method was rapid, allowing 20 samples to be analysed in 4 h.

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Section: Rh-gc Parametersmentioning

confidence: 99%

Application of programmable temperature vaporisation injection with resistive heating‐gas chromatography flame photometric detection for the determination of organophosphorus pesticides

Patel¹,

Fussell²,

Goodall

et al. 2006

J of Separation Science

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“…Modern GC -MS instruments can achieve detection limits that approach those possible with traditional selective detectors [7], and the use of large-volume injection (LVI) can further help to reduce detection limits if matrix interferences are not the limiting source of noise [2]. However, cleanup of complex extracts becomes even more important in LVI to avoid contamination of the injection liner, capillary column, and MS source with non-volatile matrix components.…”

Section: Introductionmentioning

confidence: 99%

Use of automated direct sample introduction with analyte protectants in the GC–MS analysis of pesticide residues

Čajka

Maštovská

Lehotay³

et al. 2005

J of Separation Science

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Automated large-volume direct sample introduction, or difficult matrix introduction (DMI), was investigated in the determination of 44 pesticide residues possessing a wide range of physico-chemical properties (volatility, polarity, pK(a)) in fruit-based baby food by means of gas chromatography-mass spectrometry (GC-MS) with a quadrupole mass analyzer. DMI has advantages over traditional injection because large volumes (up to 30 microL) of potentially dirty sample extracts can be injected into the GC-MS, but nonvolatile matrix components that would normally contaminate the inlet are removed after every injection. The extra matrix and glass surfaces involved in DMI, however, make the system more prone to the matrix-induced chromatographic enhancement effect, which adversely affects quantification of several pesticides. To overcome this problem, matrix-matched calibration standards and/or the use of analyte protectants were applied in the DMI approach, and the analysis of extracts was also compared before and after undergoing clean-up by dispersive solid-phase extraction. For best quantification, clean-up was still needed, and the combination of matrix-matching with analyte protectants gave the most reproducible results. Depending on the application, however, the addition of analyte protectants (a mixture of 3-ethoxy-1,2-propanediol, L-gulonic acid 3-lactone, and D-sorbitol) to sample extracts and calibration standards in solvent (non-matrix matched), gave satisfactory quantification for most of the 44 pesticides tested. The lowest calibration levels for 34 of the 44 pesticides were < or = 10 ng/g, which meets the standard required by the European Union Baby Food Directive (2003/13/EC).

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“…This type of injector may provide increased analyte detectabilities by injecting large volumes of sample. PTV large volume injection is usually conducted using the solvent split technique [7][8][9][10][11][12]. The sample is injected at an injector temperature below the solvent boiling point.…”

Section: Introductionmentioning

confidence: 99%

GC Analysis of Organic Acids and Phenols Using On-Line Methylation with Trimethylsulfonium Hydroxide and PTV Solvent Split Large Volume Injection

Zapf

Stan

1999

J. High Resol. Chromatogr.

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Large-volume injection in residue analysis with capillary gas chromatography using a conventional autosampler and injection by programmed-temperature vaporization with solvent venting

Cited by 42 publications

References 23 publications

Application of programmable temperature vaporisation injection with resistive heating‐gas chromatography flame photometric detection for the determination of organophosphorus pesticides

Application of programmable temperature vaporisation injection with resistive heating‐gas chromatography flame photometric detection for the determination of organophosphorus pesticides

Use of automated direct sample introduction with analyte protectants in the GC–MS analysis of pesticide residues

GC Analysis of Organic Acids and Phenols Using On-Line Methylation with Trimethylsulfonium Hydroxide and PTV Solvent Split Large Volume Injection

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