The determination of traces of fluoroacetic acid by extractive alkylation, pentafluorobenzylation and capillary gas chromatography-mass spectrometry

Vartiainen, Terttu; Kauranen, P.

doi:10.1016/s0003-2670(00)83609-0

Cited by 33 publications

(12 citation statements)

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“…Liquid chromatography methods have relied on fluorescence detection or tandem mass spectrometry (MS/MS) with derivatization 6–8 or without derivatization 9‐12 . GC methods based on flame ionization detection and single quadrupole MS with various types of derivatization such as alkylation with pentafluorobenzyl bromide (PFBBr), 13,14 esterification with acidic ethanol 15 and acidic n ‐propanol, 16 and coupling with 2,4‐dichloroaniline in the presence of dicyclohexylcarbodiimide 17,18 have been reported. 12 …”

Section: Introductionmentioning

confidence: 99%

“…Liquid chromatography methods have relied on fluorescence detection or tandem mass spectrometry (MS/MS) with derivatization [6][7][8] or without derivatization. [9][10][11][12] GC methods based on flame ionization detection and single quadrupole MS with various types of derivatization such as alkylation with pentafluorobenzyl bromide (PFBBr), 13,14 esterification with acidic ethanol 15 and acidic n-propanol, 16 and coupling with 2,4-dichloroaniline in the presence of dicyclohexylcarbodiimide 17,18 have been reported. 12 Here, we describe a simple modification of the aforementioned analytical techniques for the development of an easy, two-step extraction and derivatization method with well-defined, highly specific multiple reaction monitoring (MRM) transitions specific for the detection of a pentafluorobenzyl (PFB) derivative of MFA using GC/MS/MS.…”

Section: Introductionmentioning

confidence: 99%

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Pentafluorobenzylation and detection of sodium monofluoroacetate (compound 1080) in veterinary samples using gas chromatography/tandem quadrupole mass spectrometry with multiple reaction monitoring

Buchweitz

Johnson

Lehner

2021

Rapid Comm Mass Spectrometry

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The analytical detection of chemical residues from sodium monofluoroacetate (MFA) ingestion in targeted predatory wildlife and in pesticide misuse incidents perpetrated against nuisance companion animals remains a concern in veterinary forensic toxicology. There is a current need for chemically stable sample extracts with reliable and specific diagnostic methods for trace quantities in diverse diagnostic matrices. Methods: Biphasic pentafluorobenzylation provided a simple combined extraction and derivatization procedure for removing MFA in a chemically stable form from a complex matrix such as stomach contents. Analysis of the derivatized extract using gas chromatography/tandem quadrupole mass spectrometry (GC/MS/MS) with multiple reaction monitoring (MRM) approaches specific to MFA provided greater specificity than simple scan or selected ion monitoring approaches. Results: Collision-induced dissociation in GC/MS/MS showed that pentafluorobenzyl (PFB)-derivatized MFA (M + m/z 258) generated m/z 258à130, 149, 161, 177, 178, 180.1, and 181.1 transitions. Of these, the transition m/z 258à181 provided a peak for quantitation, whereas m/z 258à161 and 258à178 provided specificity for qualifying MFA. Similarly, PFB-derivatized 2-chloropropionic acid (M + m/z 288) was used as an internal standard, which generated m/z 288à181 and 161. Of these, the transition m/z 288à181 provided a peak for quantitation, whereas m/z 288à161 and 181à161 served to qualify the internal standard. Conclusions: The method was validated with a calculated limit of detection of 0.35 ppm and limit of quantitation of 1.09 ppm MFA. The method should have adequate sensitivity and reliability for veterinary toxicology labs analyzing specimens from animals poisoned by this predacide.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Pentafluorobenzylation and detection of sodium monofluoroacetate (compound 1080) in veterinary samples using gas chromatography/tandem quadrupole mass spectrometry with multiple reaction monitoring

Buchweitz

Johnson

Lehner

2021

Rapid Comm Mass Spectrometry

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“…Traditional FAA methods require a derivatization step followed by gas chromatographic (GC) separation and analysis with sensitive detection limits [5,6]. For example, Ozawa and Tsukioka report a sub-part per billion level detection limit in water [5]. However, the sample preparation procedures are extensive and time-consuming.…”

Section: Introductionmentioning

confidence: 99%

Direct aqueous injection of the fluoroacetate anion in potable water for analysis by liquid chromatography tandem mass-spectrometry

Parry

Willison

2018

Anal. Methods

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“…Lately, the efforts of these workers have focussed on the preparation of pentafluorobenzyl derivatives primarily because of the high sensitivity of the electron capture detector to derivatives of this type [12-161. This technique has been used by Vartiainen and Kauranen [17] to determine fluoroacetic acid (as the pentafluorobenzyl ester) in aqueous extracts of plant material.…”

Section: Introductionmentioning

confidence: 99%

Aqueous alkylation of anions for static headspace sampling with analysis by capillary gas chromatography‐mass spectrometry

Mulligan

1995

J Microcolumn Separations

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Abstract. The formation of ethyl derivative from anions and the conjugate bases of weak acids through the reaction with ethyl p-toluenesulfonate in strongly basic aqueous systems was used as a precursor to analysis by static headspace sampling with capillary gas chromatography-mass spectrometry. A host of materials are amenable to the technique including: cyanide, butyrate, caproate, fluoroacetate, iodide, and phenol. These analytes were used to study the performance of the system in relation to the behavior of commercially obtained ethyl derivatives. 18-Crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane) effectively catalyzes the reaction which appears to require the presence of high concentrations (5 M) of a basic salt, such as potassium carbonate. A 1:l (molar) mixture of dibasic and tribasic potassium phosphate effectively substitutes for potassium carbonate and provides improved performance for fluoroacetate while reducing interferences such as diethyl carbonate. Quantitative yields were obtained in the concentration range 0.05-2 mM, except for cyanide which produced propionitrile with an efficiency of 55580%. Fructose, at the 10% w/v level, exerted little influence upon the reaction. Calibration curves (selected ion monitoring) were linear between 0.001 and 1 mM.This approach extends the applicability of static headspace sampling and offers a potentially simple alternative to ion chromatography for complicated matrices. It should prove useful for confirming results obtained by other methods or for screening poorly characterized samples. o 1995 John Wiley & Sons, Inc.

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The determination of traces of fluoroacetic acid by extractive alkylation, pentafluorobenzylation and capillary gas chromatography-mass spectrometry

Cited by 33 publications

References 10 publications

Pentafluorobenzylation and detection of sodium monofluoroacetate (compound 1080) in veterinary samples using gas chromatography/tandem quadrupole mass spectrometry with multiple reaction monitoring

Pentafluorobenzylation and detection of sodium monofluoroacetate (compound 1080) in veterinary samples using gas chromatography/tandem quadrupole mass spectrometry with multiple reaction monitoring

Direct aqueous injection of the fluoroacetate anion in potable water for analysis by liquid chromatography tandem mass-spectrometry

Aqueous alkylation of anions for static headspace sampling with analysis by capillary gas chromatography‐mass spectrometry

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