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Fast gas chromatographic/mass spectrometric determination of diuretics and masking agents in human urine: Development and validation of a productive screening protocol for antidoping analysis.
J Chromatogr A. 2006 Dec 01; 1135(2):219-29.JC

Abstract

An analytical procedure was developed for the fast screening of 16 diuretics (acetazolamide, althiazide, amiloride, bendroflumethiazide, bumetanide, canrenoic acid, chlorthalidone, chlorthiazide, clopamide, ethacrynic acid, furosemide, hydrochlorthiazide, hydroflumethiazide, indapamide, triamterene, trichlormethiazide) and a masking agent (probenecid) in human urine. The whole method involves three analytical steps, including (1) liquid/liquid extraction of the analytes from the matrix, (2) their reaction with methyl iodide at 70 degrees C for 2 h to form methyl derivatives, (3) analysis of the resulting mixture by fast gas chromatography/electron impact mass spectrometry (fast GC/EI-MS). The analytical method was validated by determining selectivity, linearity, accuracy, intra and inter assay precision, extraction efficiencies and signal to noise ratio (S/N) at the lowest calibration level (LCL) for all candidate analytes. The analytical performances of three extraction procedures and five combination of derivatization parameters were compared in order to probe the conditions for speeding up the sample preparation step. Limits of detection (LOD) were evaluated in both EI-MS and ECNI-MS (electron capture negative ionization mass spectrometry) modes, indicating better sensitivity for most of the analytes using the latter ionization technique. The use of short columns and high carrier gas velocity in fast GC/MS produced efficient separation of the analytes in less than 4 min, resulting in a drastic reduction of the analysis time, while a resolution comparable to that obtained from classic GC conditions is maintained. Fast quadrupole MS electronics allows high scan rates and effective data acquisition both in scan and selected ion monitoring modes.

Authors+Show Affiliations

Consorzio Piemontese per la Prevenzione e Repressione del Doping e di altri Usi Illeciti dei Farmaci, Regione Gonzole 10, 10043 Orbassano, Turin, Italy.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17027009

Citation

Morra, V, et al. "Fast Gas Chromatographic/mass Spectrometric Determination of Diuretics and Masking Agents in Human Urine: Development and Validation of a Productive Screening Protocol for Antidoping Analysis." Journal of Chromatography. A, vol. 1135, no. 2, 2006, pp. 219-29.
Morra V, Davit P, Capra P, et al. Fast gas chromatographic/mass spectrometric determination of diuretics and masking agents in human urine: Development and validation of a productive screening protocol for antidoping analysis. J Chromatogr A. 2006;1135(2):219-29.
Morra, V., Davit, P., Capra, P., Vincenti, M., Di Stilo, A., & Botrè, F. (2006). Fast gas chromatographic/mass spectrometric determination of diuretics and masking agents in human urine: Development and validation of a productive screening protocol for antidoping analysis. Journal of Chromatography. A, 1135(2), 219-29.
Morra V, et al. Fast Gas Chromatographic/mass Spectrometric Determination of Diuretics and Masking Agents in Human Urine: Development and Validation of a Productive Screening Protocol for Antidoping Analysis. J Chromatogr A. 2006 Dec 1;1135(2):219-29. PubMed PMID: 17027009.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Fast gas chromatographic/mass spectrometric determination of diuretics and masking agents in human urine: Development and validation of a productive screening protocol for antidoping analysis. AU - Morra,V, AU - Davit,P, AU - Capra,P, AU - Vincenti,M, AU - Di Stilo,A, AU - Botrè,F, Y1 - 2006/10/05/ PY - 2006/04/10/received PY - 2006/09/07/revised PY - 2006/09/15/accepted PY - 2006/10/10/pubmed PY - 2007/1/5/medline PY - 2006/10/10/entrez SP - 219 EP - 29 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1135 IS - 2 N2 - An analytical procedure was developed for the fast screening of 16 diuretics (acetazolamide, althiazide, amiloride, bendroflumethiazide, bumetanide, canrenoic acid, chlorthalidone, chlorthiazide, clopamide, ethacrynic acid, furosemide, hydrochlorthiazide, hydroflumethiazide, indapamide, triamterene, trichlormethiazide) and a masking agent (probenecid) in human urine. The whole method involves three analytical steps, including (1) liquid/liquid extraction of the analytes from the matrix, (2) their reaction with methyl iodide at 70 degrees C for 2 h to form methyl derivatives, (3) analysis of the resulting mixture by fast gas chromatography/electron impact mass spectrometry (fast GC/EI-MS). The analytical method was validated by determining selectivity, linearity, accuracy, intra and inter assay precision, extraction efficiencies and signal to noise ratio (S/N) at the lowest calibration level (LCL) for all candidate analytes. The analytical performances of three extraction procedures and five combination of derivatization parameters were compared in order to probe the conditions for speeding up the sample preparation step. Limits of detection (LOD) were evaluated in both EI-MS and ECNI-MS (electron capture negative ionization mass spectrometry) modes, indicating better sensitivity for most of the analytes using the latter ionization technique. The use of short columns and high carrier gas velocity in fast GC/MS produced efficient separation of the analytes in less than 4 min, resulting in a drastic reduction of the analysis time, while a resolution comparable to that obtained from classic GC conditions is maintained. Fast quadrupole MS electronics allows high scan rates and effective data acquisition both in scan and selected ion monitoring modes. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17027009/Fast_gas_chromatographic/mass_spectrometric_determination_of_diuretics_and_masking_agents_in_human_urine:_Development_and_validation_of_a_productive_screening_protocol_for_antidoping_analysis_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(06)01791-2 DB - PRIME DP - Unbound Medicine ER -