Evolving criteria for confirmation of trace level residues in food and drugs by mass spectrometry. Part II

Cairns, Thomas; Siegmund, Emil G.; Stamp, John J.

doi:10.1002/mas.1280080302

Cited by 10 publications

(3 citation statements)

References 57 publications

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“…[49][50][51][52][53][54][55][56][57] A number of reviews describing the development of criteria for confirmation using GC/MS, LC/MS, and MS/MS have been published. [58][59][60][61] The original guideline of a minimum of three ions for confirmation has been widely adopted. Today, the majority of confirmations reported in the literature have been performed with three or more ions.…”

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confidence: 99%

“…However, a number of factors have been commonly used in the literature as proof for confirmation since Sphon in 1978 48 defined specific requirements for the confirmation of drug residues by GC/electron impact MS. These factors include the matching of the compound retention time with a standard and the presence of three or more characteristic ions with the appropriate relative abundance compared to a standard. − A number of reviews describing the development of criteria for confirmation using GC/MS, LC/MS, and MS/MS have been published. − The original guideline of a minimum of three ions for confirmation has been widely adopted. Today, the majority of confirmations reported in the literature have been performed with three or more ions.…”

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confidence: 99%

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Confirmation and Quantitation of Selected Sulfonylurea, Imidazolinone, and Sulfonamide Herbicides in Surface Water Using Electrospray LC/MS

1998

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A multianalyte method has been developed for the confirmation and quantitation of 16 selected sulfonylurea, imidazolinone, and sulfonamide herbicides in surface water. Samples are acidified, the analytes are extracted using RP-102 extraction cartridges, and the extracts are cleaned-up using an anion-exchange cartridge (SAX) stacked on top of an alumina cartridge. The final extracts are evaporated to dryness, redissolved in 10:90 or 20:80 acetonitrile/water, and analyzed using electrospray LC/MS. Confirmation criteria were defined so that identification of the analytes could be made with a reasonable degree of scientific certainty. Confirmation required that (1) LC/MS retention times of the analytes be within 1% of the retention times of the standards, (2) the molecular ion and two characteristic fragment ions per analyte be present, and (3) ion abundance ratios of the fragment ions relative to the molecular ion be within 20% of the ion ratios obtained for the standards. Each of the analytes in all of the samples used to validate this method met these confirmation criteria. Quantitation of the analytes at 0.1 and 1.0 ppb was demonstrated, with average recoveries between 70% and 114% and relative standard deviations that were less than 13%. The limit of quantitation (LOQ) for this method is 0.1 ppb (ng/mL) for all analytes. Six water types were used for the validation of this method.

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Confirmation and Quantitation of Selected Sulfonylurea, Imidazolinone, and Sulfonamide Herbicides in Surface Water Using Electrospray LC/MS

1998

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“…Chemical ionization of pesticides Chemical ionization (Cl) techniques to favor the production of a protonated molecular ion for characterization have been the cornerstone of resolving both the identification and confirmation of pesticide residues over the past decade (10). The power behind this strategy is based on the fact that under Cl only a few fragment ions, in addition to the protonated molecule ion, appear in the mass spectrum.…”

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confidence: 99%

Pesticide analysis in food by MS

Cairns¹,

Baldwin²

1995

Anal. Chem.

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Multi-residue confirmation of aminoglycoside antibiotics and bovine kidney by ion spray high-performance liquid chromatography/tandem mass spectrometry

McLaughlin

Henion

Kijak³

1994

Biol. Mass Spectrom.

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An ion spray high-performance liquid chromatographic/tandem mass spectrometric (HPLC/MS/MS) method capable of determining the following six aminoglycosides in bovine kidney is presented: spectinomycin, hygromycin B, streptomycin, dihydrostreptomycin, gentamicin C complex and neomycin B. Tobramycin was used as an internal standard. This method uses an improved matrix solid-phase dispersion (MSPD) method for tissue extraction. A gradient HPLC separation was developed with mobile phases consisting of aqueous 20 mM pentafluoropropionic acid and acetonitrile. Protonated molecules served as precursor ions for collision-induced dissociation (CID) and three product ions were chosen for each analyte for selected reaction monitoring (SRM) where possible. A validation study was conducted for the confirmation of dihydrostreptomycin, neomycin B and four major components of the gentamicin C complex through SRM HPLC/MS/MS analysis of negative control, fortified and incurred bovine kidney samples. All of the samples analyzed could be confirmed with ion ratios within 15% of the daily mean of fortified standards and 90% of the samples had ion ratios within 10%. All compounds except spectinomycin could be detected (while monitoring three ions by SRM) in bovine kidney tissue at or below the regulatory level of concern. MSPD recoveries were acceptable with the exception of the 27% value observed for spectinomycin.

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Evolving criteria for confirmation of trace level residues in food and drugs by mass spectrometry. Part II

Cited by 10 publications

References 57 publications

Confirmation and Quantitation of Selected Sulfonylurea, Imidazolinone, and Sulfonamide Herbicides in Surface Water Using Electrospray LC/MS

Confirmation and Quantitation of Selected Sulfonylurea, Imidazolinone, and Sulfonamide Herbicides in Surface Water Using Electrospray LC/MS

Pesticide analysis in food by MS

Multi-residue confirmation of aminoglycoside antibiotics and bovine kidney by ion spray high-performance liquid chromatography/tandem mass spectrometry

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