Detection and quantification of lanosterol and dihydrolanosterol esters by measurements of metastable decompositions. Application to their direct analysis in wool wax

Patouraux, D.; Lacave, Charlotte; Promé, Jean‐Claude

doi:10.1002/bms.1200080307

Cited by 4 publications

(2 citation statements)

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“…Two direct coupling interfaces for micro high-performance ILC/M!3s have been described, with the acetonitrile solvents also functioning as chemical ionization reagent gases. Steroids (056) and polycyclic aromatic hydrocarbons (057) were used to illustrate the performance of these two interfaces. The direct coupling of a supercritical gas chromatograph t,o a mass spectrometer using a supersonic molecular beam interface has been fabricated capable of chromatographic pressures of at least 300 atm and temperatures from 10 to 60 OC (058).…”

Section: Spectrometric/on-line Computermentioning

confidence: 99%

“…Gaskell and Pike have reviewed the principles of this technique (053) which has been further developed to allow multiple metastable peak monitoring (054). The technique has been applied to the analysis of steroids in saliva in the concentration range 20 pg mL-l to 20 ng mL,-l (055), to the quantitation of androstanolones as their methyloxime tert-butyldimethylsilyl ether derivatives (056), and to the detection and quantitation of lanosterol and dihydrolanosterol esters in wool wax (057).…”

Section: Steroids Sterols and Bile Acidsmentioning

confidence: 99%

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Mass spectrometry

Burlingame¹,

Dell²,

Russell³

1982

Anal. Chem.

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37bb) Viswanatha, V.; Larsen, 8.; Hruby, V. J. Tetrahedron 1979, 35, (38bb) Zolotarev. Yu. A.; Myasoedov, N. F.; Penkina, V. I.; Petrenik, 0. R.; Process LC (lcc) Bade, R. K.; Benningfield, L. V., Jr.; Mowery, R. A., Jr.; Fuller, E. N. (2cc) Benningfield, I_. V., Jr.; Mowery, R. A,, Jr. J . Chromatogr. Sci. 1981, (3cc) Broerman, A. 6.; Mowery, R. A,, Jr. (3dd) Briggie, T. V.; Allen, L. M.; Duncan, R. C.; Pfaffenberger, C. D. J . (4dd) Janssens. G. HRCCC, J . High Resoiut. Chromatogr ., Chromatogr. (5dd) Karmen, A.; Lam, S.; Cummings, G.; Chow, F. J . Chromatogr. 1980, (6dd) Kobayashi, 0.; Matsui, K.; Minamlura, N.; Yamamoto, T. J . Chroma-(7dd) Lafont, R.; Beydon, P.; Somme-Martin, G.; Blais, C. Steroids 1980, 38, (8dd) Lal, C.-C.; Lin, J.-K. K'o Hsueh Fa Chan Yueh K'an 1980, 8 , 941-955 (9dd) McGuffin, V. L.; Novotny, M. Anal. Chem. 1981, 53, 946-951. (10dd) Okada, K.; Taneka, J.; Miyashita, A,; Imoto, K. Yakugaku Zatrshi (lldd) Paik, N. H.; Park, M. K.; Park, J. H.; Klm, C. S.; Suh, J. J. YakhakHoe (12dd) Resha, M.; Langley, D.; Eisenstadt, E. Mutat. Res. 1981, 85, 97-108. (13dd) Reuiand, D. J.; Trinler, W. A. J. Forensic Sci. SOC. 1980, 20, (14dd) Serban, M.; Gozia, 0. Rev. Roum. Biochim. 1980, 77, 145-152. (15dd) Stewart, R. N.; Asen, S.; Massle, D. R.; Norris, K. H. Biochem. Syst. 355-360. OVERVIEWThe instrumental methods that comprise mass spectrometry are preeminent in the experimental investigation of the molecular nature of matter, since the measured parameters in true gas-phase mass spectrometry relate directly to chemical reactions of the substance in question. These reactions can be controlled by the mode of their production and in some cases the reactive molecular species can be formed with a narrow distribution of internal energies. All the products of such reactions, including their nuclidic composition, are measured essentially simultaneously and can be related to the structure (and stereochemistry) of the neutral species under investigation. These techniques operate with extreme sensitivity, unrivaled by electromagnetic spectroscopic techniques, and maintain an inherent substance specificity during measurement. The observables-the mass spectrometric information-are defined by the chemical reactivity of internally energized molecules.As a point of embarkation in consideration of the nature of less well understood processes operative in the newer "surface desorption" ion sources, on the one hand it is well established that field ionized molecular ions display true unimolecular dissociation from intramolecular reaction processes outside the high field gradient ( , .. 100 A from emitter tip), except that their maximum range of internal energy is low, viz., comparable to 12 eV electron impact (AI). However, even with this technique, certain processes observed in the "normal" field ionization mass spectrum are induced only by molecular interaction on the emitter surface (AZ). As one considers more intimate possible interactions of labile biological sample with surfaces of varying composition and chemic...

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Section: Spectrometric/on-line Computermentioning

confidence: 99%

Section: Steroids Sterols and Bile Acidsmentioning

confidence: 99%

Mass spectrometry

Burlingame¹,

Dell²,

Russell³

1982

Anal. Chem.

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Detection and quantification of steroids produced by microbial fermentation of sterols by means of MIKE spectrometry and selected Metastable Ion Monitoring

Promé

Lacave

Roussel

et al. 1982

Biol. Mass Spectrom.

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Several steroids generated by microbial fermentation of cholesterol were identified by the mass analysed ion kinetic energy (MIKE) spectra of their molecular ions generated under electron impact, and quantified by selected metastable ion monitoring. These analyses were performed on a crude solvent extract without any purification or molecular separation procedures. The detection limit was below the nanogram range. Identification and quantification of the major constituents, namely androst-4-ene-3,17-dione and androsta-1,4-diene-3,17-dione were fast and easy. Pregnenolone and progesterone which were present at a much lower level were identified with more difficulty by their MIKE spectra alone, because of the existence of isobaric interfering ions. Nevertheless, their quantification by single or dual metastable monitoring was possible.

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