Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods
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2015
Authors
Kostić, NadaDotsikas, Yannis
Jović, Nebojša
Stevanović, Galina
Malenović, Anđelija
Medenica, Mirjana
Article (Published version)
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In this paper, novel LC-MS/MS methods for the determination of antiepileptic drug pregabalin in dried matrix spots (DMS) are presented. This attractive technique of sample collection in micro amount was utilized in the form of dried blood spots (DBS) and dried plasma spots (DPS). Following a pre-column derivatization procedure, using n-propyl chloroformate in the presence of n-propanol, and consecutive liquid-liquid extraction, derivatized pregabalin and its internal standard, 4-aminocyclohexanecarboxylic acid, were detected in positive ion mode by applying two SRM transitions per analyte. A YMC-Pack Octyl column (50 mm x 4.0 mm, 3 mu m particle size) maintained at 30 degrees C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550 mu L/min and total run time 2 min. Established methods were fully validated over the concentration range of 0.200-20.0 mu g/mL for DBS and 0.400-40.0 mu g/mL for DPS, respectively, while specificit...y, accuracy, precision, recovery, matrix-effect, stability, dilution integrity and spot homogeneity were found within acceptance criteria. Validated methods were applied for the determination of pregabalin levels in dried blood and plasma samples obtained from patients with epilepsy, after per os administration of commercial capsules. Comparison of drug level in blood and plasma, as well as correction steps undertaken in order to overcome hematocrit issue, when analyzing DBS, are also given.
Keywords:
Pregabalin / Chloroformates / Dried blood/plasma spots / Mass spectrometry / HematocritSource:
Journal of Pharmaceutical and Biomedical Analysis, 2015, 109, 79-84Publisher:
- Elsevier Science BV, Amsterdam
Funding / projects:
- Modelling of different chromatographic systems with chemometrical approach in pharmaceutical analysis (RS-MESTD-Basic Research (BR or ON)-172052)
DOI: 10.1016/j.jpba.2015.02.023
ISSN: 0731-7085
PubMed: 25767905
WoS: 000353078700011
Scopus: 2-s2.0-84924370331
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PharmacyTY - JOUR AU - Kostić, Nada AU - Dotsikas, Yannis AU - Jović, Nebojša AU - Stevanović, Galina AU - Malenović, Anđelija AU - Medenica, Mirjana PY - 2015 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/2410 AB - In this paper, novel LC-MS/MS methods for the determination of antiepileptic drug pregabalin in dried matrix spots (DMS) are presented. This attractive technique of sample collection in micro amount was utilized in the form of dried blood spots (DBS) and dried plasma spots (DPS). Following a pre-column derivatization procedure, using n-propyl chloroformate in the presence of n-propanol, and consecutive liquid-liquid extraction, derivatized pregabalin and its internal standard, 4-aminocyclohexanecarboxylic acid, were detected in positive ion mode by applying two SRM transitions per analyte. A YMC-Pack Octyl column (50 mm x 4.0 mm, 3 mu m particle size) maintained at 30 degrees C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550 mu L/min and total run time 2 min. Established methods were fully validated over the concentration range of 0.200-20.0 mu g/mL for DBS and 0.400-40.0 mu g/mL for DPS, respectively, while specificity, accuracy, precision, recovery, matrix-effect, stability, dilution integrity and spot homogeneity were found within acceptance criteria. Validated methods were applied for the determination of pregabalin levels in dried blood and plasma samples obtained from patients with epilepsy, after per os administration of commercial capsules. Comparison of drug level in blood and plasma, as well as correction steps undertaken in order to overcome hematocrit issue, when analyzing DBS, are also given. PB - Elsevier Science BV, Amsterdam T2 - Journal of Pharmaceutical and Biomedical Analysis T1 - Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods VL - 109 SP - 79 EP - 84 DO - 10.1016/j.jpba.2015.02.023 ER -
@article{ author = "Kostić, Nada and Dotsikas, Yannis and Jović, Nebojša and Stevanović, Galina and Malenović, Anđelija and Medenica, Mirjana", year = "2015", abstract = "In this paper, novel LC-MS/MS methods for the determination of antiepileptic drug pregabalin in dried matrix spots (DMS) are presented. This attractive technique of sample collection in micro amount was utilized in the form of dried blood spots (DBS) and dried plasma spots (DPS). Following a pre-column derivatization procedure, using n-propyl chloroformate in the presence of n-propanol, and consecutive liquid-liquid extraction, derivatized pregabalin and its internal standard, 4-aminocyclohexanecarboxylic acid, were detected in positive ion mode by applying two SRM transitions per analyte. A YMC-Pack Octyl column (50 mm x 4.0 mm, 3 mu m particle size) maintained at 30 degrees C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550 mu L/min and total run time 2 min. Established methods were fully validated over the concentration range of 0.200-20.0 mu g/mL for DBS and 0.400-40.0 mu g/mL for DPS, respectively, while specificity, accuracy, precision, recovery, matrix-effect, stability, dilution integrity and spot homogeneity were found within acceptance criteria. Validated methods were applied for the determination of pregabalin levels in dried blood and plasma samples obtained from patients with epilepsy, after per os administration of commercial capsules. Comparison of drug level in blood and plasma, as well as correction steps undertaken in order to overcome hematocrit issue, when analyzing DBS, are also given.", publisher = "Elsevier Science BV, Amsterdam", journal = "Journal of Pharmaceutical and Biomedical Analysis", title = "Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods", volume = "109", pages = "79-84", doi = "10.1016/j.jpba.2015.02.023" }
Kostić, N., Dotsikas, Y., Jović, N., Stevanović, G., Malenović, A.,& Medenica, M.. (2015). Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods. in Journal of Pharmaceutical and Biomedical Analysis Elsevier Science BV, Amsterdam., 109, 79-84. https://doi.org/10.1016/j.jpba.2015.02.023
Kostić N, Dotsikas Y, Jović N, Stevanović G, Malenović A, Medenica M. Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods. in Journal of Pharmaceutical and Biomedical Analysis. 2015;109:79-84. doi:10.1016/j.jpba.2015.02.023 .
Kostić, Nada, Dotsikas, Yannis, Jović, Nebojša, Stevanović, Galina, Malenović, Anđelija, Medenica, Mirjana, "Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods" in Journal of Pharmaceutical and Biomedical Analysis, 109 (2015):79-84, https://doi.org/10.1016/j.jpba.2015.02.023 . .