Mass spectrometric determination of n-hydroxyphenacetin in urine using multiple metastable peak monitoring following thin-layer chromatography

Davies, Noel W.; Veronese, Maurice E.; McLean, Stuart

doi:10.1016/0378-4347(84)80079-1

Cited by 9 publications

(2 citation statements)

References 18 publications

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“…The metabolism of steroids in several different animal species was followed with TLC sample preparation, spot extraction, and highresolution mass spectrometry (20). The metabolites of phenacetin in urine (21) and identification of a number of drugs given to racehorses has also been accomplished with a combination of thinlayer chromatography and mass spectrometry (22). Metabolites of the carcinogen 7-methylbenz[c]acridine were separated by TLC and high-performance LC and subsequently characterized by mass spectrometry (23).…”

Section: Extraction Of Sample Spots From Adsorbentsmentioning

confidence: 99%

Thin-Layer Chromatography Coupled with Mass Spectrometry

Busch¹

2003

Handbook of Thin-Layer Chromatography

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Section: Extraction Of Sample Spots From Adsorbentsmentioning

confidence: 99%

Thin-Layer Chromatography Coupled with Mass Spectrometry

Busch¹

2003

Handbook of Thin-Layer Chromatography

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“…The first involves scraping the analyte spot from the plate and extracting into a solvent. The extracted analyte is then analyzed by MS in a conventional manner [3,4]. A second method involves analysis of a small piece of TLC cut from the plate.…”

Section: Introductionmentioning

confidence: 99%

Coupling protocol for thin layer chromatography/matrix-assisted laser desorption ionization

1997

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SummaryThis paper reports the investigation and optimization of the thin layer chromatography/matrix-assisted laser desorption/ionization (TLC-MALDI) coupling protocol. The fundamental coupling parameters which influence sensitivity and lateral analyte spreading are extraction solvent selection, extraction time, and pressure. Selection of the solvent is dependent upon its extraction efficiency, which has been correlated with extraction solvent Rf value. Maximum extraction efficiency occurs after two minutes for the analyte/solvent system studied. High extraction efficiency solvents cause significant lateral spreading of analyte; up to a three-fold increase in initial analyte spot size. Analyte recovery was found to be limited by the silica gel inter-particle porosity and the solvent extraction efficiency. For maintaining chromatographic resolution and maximizing signal intensity, extraction solvents with Rf values between 0.4 to 0.6 are optimal. The upper analyte recovery limit, using extraction solvents within this Rf range, is estimated at 22 %.

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Selected reaction monitoring during gas chromatography/mass spectrometry of eicosanoids

Hughes¹,

Nowlin²,

Gaskell³

et al. 1988

Biol. Mass Spectrom.

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Gas chromatography/electron capture negative ion mass spectrometry of eicosanoids, as pentafluorobenzyl (PFB) ester, methyl oxime (where applicable), trimethylsilyl (TMS) ether derivatives, is reported using a double-focusing instrument of trisector configuration. Sub-picogram detection limits were observed for prostaglandins E1, E2 and F2 alpha during selected ion monitoring (SIM) of [M-PFB]- ions. Selected reaction monitoring (SRM) of [M-PFB]-----[M-PFB-TMSOH]-, occurring in the first field-free region, was of modest sensitivity, reflecting the stability of the [M-PFB]- ions. The leukotriene B4 (LTB4) derivative was successfully analyzed by SIM at the low-picogram level. In this instance, the fragmentation [M-PFB]-----[M-PFB-TMSOH] occurred in high yield in the first field-free region. The advantageous improvement in selectivity of detection that may be achieved with SRM was evident during the analysis of a serum extract for LTB4.

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Mass spectrometric determination of n-hydroxyphenacetin in urine using multiple metastable peak monitoring following thin-layer chromatography

Cited by 9 publications

References 18 publications

Thin-Layer Chromatography Coupled with Mass Spectrometry

Thin-Layer Chromatography Coupled with Mass Spectrometry

Coupling protocol for thin layer chromatography/matrix-assisted laser desorption ionization

Selected reaction monitoring during gas chromatography/mass spectrometry of eicosanoids

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