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Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine.
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Feb 01; 877(4):369-74.JC

Abstract

The objective of this study was to develop a simple and robust LC-MS/MS method for the quantification of ephedrine type substances in urine. Sample preparation consisted of a 10-fold dilution step of the samples into the internal standard solution (ephedrine-d(3), 4 microg/mL in water). Baseline separation of the diastereoisomers norpseudoephedrine-norephedrine and ephedrine-pseudoephedrine was performed on a C8-column using isocratic conditions followed by positive electrospray ionisation and tandem mass spectrometric detection. The mobile phase consisted of 98/2 (H(2)O/ACN) containing 0.1% HAc and 0.01% TFA. Calibration curves were constructed between 2.5 and 10 microg/mL for norephedrine and norpseudoephedrine and 5 and 20 microg/mL for ephedrine, pseudoephedrine and methylephedrine. The bias ranged from -5.5 to 12% for norephedrine, -4.1 to 8.0 % for norpseudoephedrine, 0.3 to 2.1 % for ephedrine, 1.6 to 2.6 % for pseudoephedrine and 2.9 to 5.0 % for methylephedrine. Precision of the method varied between 2.8 and 10.4% for all compounds and the matrix effect was less than 15%. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-NPD method. Results show a good correlation between both methods with correlation coefficients higher than 0.95 for all analytes.

Authors+Show Affiliations

DoCoLab, UGent, Department of Clinical Chemistry, Microbiology and Immunology, Technologiepark 30, B-9052 Zwijnaarde, Belgium. Koen.Deventer@UGent.beNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

19144576

Citation

Deventer, K, et al. "Development and Validation of an LC-MS/MS Method for the Quantification of Ephedrines in Urine." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 877, no. 4, 2009, pp. 369-74.
Deventer K, Pozo OJ, Van Eenoo P, et al. Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2009;877(4):369-74.
Deventer, K., Pozo, O. J., Van Eenoo, P., & Delbeke, F. T. (2009). Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 877(4), 369-74. https://doi.org/10.1016/j.jchromb.2008.12.032
Deventer K, et al. Development and Validation of an LC-MS/MS Method for the Quantification of Ephedrines in Urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Feb 1;877(4):369-74. PubMed PMID: 19144576.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and validation of an LC-MS/MS method for the quantification of ephedrines in urine. AU - Deventer,K, AU - Pozo,O J, AU - Van Eenoo,P, AU - Delbeke,F T, Y1 - 2008/12/24/ PY - 2008/10/06/received PY - 2008/12/08/revised PY - 2008/12/14/accepted PY - 2009/1/16/entrez PY - 2009/1/16/pubmed PY - 2009/4/8/medline SP - 369 EP - 74 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 877 IS - 4 N2 - The objective of this study was to develop a simple and robust LC-MS/MS method for the quantification of ephedrine type substances in urine. Sample preparation consisted of a 10-fold dilution step of the samples into the internal standard solution (ephedrine-d(3), 4 microg/mL in water). Baseline separation of the diastereoisomers norpseudoephedrine-norephedrine and ephedrine-pseudoephedrine was performed on a C8-column using isocratic conditions followed by positive electrospray ionisation and tandem mass spectrometric detection. The mobile phase consisted of 98/2 (H(2)O/ACN) containing 0.1% HAc and 0.01% TFA. Calibration curves were constructed between 2.5 and 10 microg/mL for norephedrine and norpseudoephedrine and 5 and 20 microg/mL for ephedrine, pseudoephedrine and methylephedrine. The bias ranged from -5.5 to 12% for norephedrine, -4.1 to 8.0 % for norpseudoephedrine, 0.3 to 2.1 % for ephedrine, 1.6 to 2.6 % for pseudoephedrine and 2.9 to 5.0 % for methylephedrine. Precision of the method varied between 2.8 and 10.4% for all compounds and the matrix effect was less than 15%. The applicability of the method has been checked by the analysis of 40 urine samples. The results were compared with those obtained with the common GC-NPD method. Results show a good correlation between both methods with correlation coefficients higher than 0.95 for all analytes. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/19144576/Development_and_validation_of_an_LC_MS/MS_method_for_the_quantification_of_ephedrines_in_urine_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(08)00928-8 DB - PRIME DP - Unbound Medicine ER -