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Gas chromatographic-mass spectrometric determination of serum mexiletine concentration after derivatization with perfluorooctanoyl chloride, a new derivative.
J Chromatogr B Biomed Sci Appl. 1998 Feb 13; 705(2):283-8.JC

Abstract

Mexiletine is an antiarrhythmic agent used in the treatment of ventricular arrhythmia. The drug has a narrow therapeutic window which necessitates monitoring its serum concentrations. We describe a gas chromatographic-mass spectrometric analysis of mexiletine using selected ion monitoring. Mexiletine was extracted from alkaline serum with dichloromethane and then derivatized with perfluorooctanoyl chloride. The derivatization reaction was completed in 20 min at 80 degrees C. We used N-propylamphetamine as the internal standard. The ions monitored were m/z 122, 454 and 575 for the derivatized mexiletine and m/z 91, 118, 440 and 452 for the derivatized internal standard. The within-run precision at a serum mexiletine concentration of 1 mg/l was 1.9% (mean=0.98, S.D.=0.019 mg/l, n=7) and the between-run precision was 2.5% (mean=0.99, S.D.=0.025 mg/l, n=7). The assay was linear for serum mexiletine concentrations of 0.2 to 4 mg/l. The detection limit was 0.1 mg/l. The average recoveries of mexiletine and the internal standard were 80% and 84%, respectively at a mexiletine concentration of 1 mg/l. There was no carry over problem in our assay. We observed a good correlation between mexiletine concentrations measured by a reference laboratory (GC) and by our new GC-MS assay.

Authors+Show Affiliations

Department of Pathology, University of New Mexico Health Sciences Center, Albuquerque 87106, USA.No affiliation info available

Pub Type(s)

Comparative Study
Journal Article

Language

eng

PubMed ID

9521565

Citation

Dasgupta, A, and O Yousef. "Gas Chromatographic-mass Spectrometric Determination of Serum Mexiletine Concentration After Derivatization With Perfluorooctanoyl Chloride, a New Derivative." Journal of Chromatography. B, Biomedical Sciences and Applications, vol. 705, no. 2, 1998, pp. 283-8.
Dasgupta A, Yousef O. Gas chromatographic-mass spectrometric determination of serum mexiletine concentration after derivatization with perfluorooctanoyl chloride, a new derivative. J Chromatogr B Biomed Sci Appl. 1998;705(2):283-8.
Dasgupta, A., & Yousef, O. (1998). Gas chromatographic-mass spectrometric determination of serum mexiletine concentration after derivatization with perfluorooctanoyl chloride, a new derivative. Journal of Chromatography. B, Biomedical Sciences and Applications, 705(2), 283-8.
Dasgupta A, Yousef O. Gas Chromatographic-mass Spectrometric Determination of Serum Mexiletine Concentration After Derivatization With Perfluorooctanoyl Chloride, a New Derivative. J Chromatogr B Biomed Sci Appl. 1998 Feb 13;705(2):283-8. PubMed PMID: 9521565.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Gas chromatographic-mass spectrometric determination of serum mexiletine concentration after derivatization with perfluorooctanoyl chloride, a new derivative. AU - Dasgupta,A, AU - Yousef,O, PY - 1998/4/1/pubmed PY - 1998/4/1/medline PY - 1998/4/1/entrez SP - 283 EP - 8 JF - Journal of chromatography. B, Biomedical sciences and applications JO - J. Chromatogr. B Biomed. Sci. Appl. VL - 705 IS - 2 N2 - Mexiletine is an antiarrhythmic agent used in the treatment of ventricular arrhythmia. The drug has a narrow therapeutic window which necessitates monitoring its serum concentrations. We describe a gas chromatographic-mass spectrometric analysis of mexiletine using selected ion monitoring. Mexiletine was extracted from alkaline serum with dichloromethane and then derivatized with perfluorooctanoyl chloride. The derivatization reaction was completed in 20 min at 80 degrees C. We used N-propylamphetamine as the internal standard. The ions monitored were m/z 122, 454 and 575 for the derivatized mexiletine and m/z 91, 118, 440 and 452 for the derivatized internal standard. The within-run precision at a serum mexiletine concentration of 1 mg/l was 1.9% (mean=0.98, S.D.=0.019 mg/l, n=7) and the between-run precision was 2.5% (mean=0.99, S.D.=0.025 mg/l, n=7). The assay was linear for serum mexiletine concentrations of 0.2 to 4 mg/l. The detection limit was 0.1 mg/l. The average recoveries of mexiletine and the internal standard were 80% and 84%, respectively at a mexiletine concentration of 1 mg/l. There was no carry over problem in our assay. We observed a good correlation between mexiletine concentrations measured by a reference laboratory (GC) and by our new GC-MS assay. SN - 1387-2273 UR - https://www.unboundmedicine.com/medline/citation/9521565/Gas_chromatographic_mass_spectrometric_determination_of_serum_mexiletine_concentration_after_derivatization_with_perfluorooctanoyl_chloride_a_new_derivative_ DB - PRIME DP - Unbound Medicine ER -