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Development and validation of a selective and robust LC-MS/MS method for high-throughput quantifying rizatriptan in small plasma samples: application to a clinical pharmacokinetic study.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Dec 05; 844(2):268-77.JC

Abstract

An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection (LC-MS/MS) was developed for the determination of a potent 5-HT(1B/1D) receptor agonist, rizatriptan in human plasma using granisetron as the internal standard. The analyte and internal standard were isolated from 100 microL plasma samples by liquid-liquid extraction (LLE) and chromatographed on a Lichrospher C18 column (4.6mm x 50mm, 5 microm) with a mobile phase consisting of acetonitrile-10mM aqueous ammonium acetate-acetic acid (50:50:0.5, v/v/v) pumped at 1.0 mL/min. The method had a chromatographic total run time of 2 min. A Varian 1200 L electrospray tandem mass spectrometer equipped with an electrospray ionization source was operated in selected reaction monitoring (SRM) mode with the precursor-to-product ion transitions m/z 270-->201 (rizatriptan) and 313.4-->138 (granisetron) used for quantitation. The assay was validated over the concentration range of 0.05-50 ng/mL and was found to have acceptable accuracy, precision, linearity, and selectivity. The mean extraction recovery from spiked plasma samples was above 98%. The intra-day accuracy of the assay was within 12% of nominal and intra-day precision was better than 13% C.V. Following a 10mg dose of the compound administered to human subjects, mean concentrations of rizatriptan ranged from 0.2 to 70.6 ng/mL in plasma samples collected up to 24h after dosing. Inter-day accuracy and precision results for quality control samples run over a 5-day period alongside clinical samples showed mean accuracies of within 12% of nominal and precision better than 9.5% C.V.

Authors+Show Affiliations

Department of Pharmaceutical Analysis, School of Pharmacy, Second Military Medical University, No. 325 Guohe Road, Shanghai 200433, PR China.No affiliation info availableNo 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
Validation Study

Language

eng

PubMed ID

16899417

Citation

Chen, Yi, et al. "Development and Validation of a Selective and Robust LC-MS/MS Method for High-throughput Quantifying Rizatriptan in Small Plasma Samples: Application to a Clinical Pharmacokinetic Study." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 844, no. 2, 2006, pp. 268-77.
Chen Y, Miao H, Lin M, et al. Development and validation of a selective and robust LC-MS/MS method for high-throughput quantifying rizatriptan in small plasma samples: application to a clinical pharmacokinetic study. J Chromatogr B Analyt Technol Biomed Life Sci. 2006;844(2):268-77.
Chen, Y., Miao, H., Lin, M., Fan, G., Hong, Z., Wu, H., & Wu, Y. (2006). Development and validation of a selective and robust LC-MS/MS method for high-throughput quantifying rizatriptan in small plasma samples: application to a clinical pharmacokinetic study. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 844(2), 268-77.
Chen Y, et al. Development and Validation of a Selective and Robust LC-MS/MS Method for High-throughput Quantifying Rizatriptan in Small Plasma Samples: Application to a Clinical Pharmacokinetic Study. J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Dec 5;844(2):268-77. PubMed PMID: 16899417.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and validation of a selective and robust LC-MS/MS method for high-throughput quantifying rizatriptan in small plasma samples: application to a clinical pharmacokinetic study. AU - Chen,Yi, AU - Miao,Haijun, AU - Lin,Mei, AU - Fan,Guorong, AU - Hong,Zhanying, AU - Wu,Huiling, AU - Wu,Yutian, Y1 - 2006/08/08/ PY - 2006/01/19/received PY - 2006/06/29/revised PY - 2006/07/15/accepted PY - 2006/8/11/pubmed PY - 2007/1/17/medline PY - 2006/8/11/entrez SP - 268 EP - 77 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 844 IS - 2 N2 - An analytical method based on liquid chromatography with positive ion electrospray ionization (ESI) coupled to tandem mass spectrometry detection (LC-MS/MS) was developed for the determination of a potent 5-HT(1B/1D) receptor agonist, rizatriptan in human plasma using granisetron as the internal standard. The analyte and internal standard were isolated from 100 microL plasma samples by liquid-liquid extraction (LLE) and chromatographed on a Lichrospher C18 column (4.6mm x 50mm, 5 microm) with a mobile phase consisting of acetonitrile-10mM aqueous ammonium acetate-acetic acid (50:50:0.5, v/v/v) pumped at 1.0 mL/min. The method had a chromatographic total run time of 2 min. A Varian 1200 L electrospray tandem mass spectrometer equipped with an electrospray ionization source was operated in selected reaction monitoring (SRM) mode with the precursor-to-product ion transitions m/z 270-->201 (rizatriptan) and 313.4-->138 (granisetron) used for quantitation. The assay was validated over the concentration range of 0.05-50 ng/mL and was found to have acceptable accuracy, precision, linearity, and selectivity. The mean extraction recovery from spiked plasma samples was above 98%. The intra-day accuracy of the assay was within 12% of nominal and intra-day precision was better than 13% C.V. Following a 10mg dose of the compound administered to human subjects, mean concentrations of rizatriptan ranged from 0.2 to 70.6 ng/mL in plasma samples collected up to 24h after dosing. Inter-day accuracy and precision results for quality control samples run over a 5-day period alongside clinical samples showed mean accuracies of within 12% of nominal and precision better than 9.5% C.V. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/16899417/Development_and_validation_of_a_selective_and_robust_LC_MS/MS_method_for_high_throughput_quantifying_rizatriptan_in_small_plasma_samples:_application_to_a_clinical_pharmacokinetic_study_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(06)00590-3 DB - PRIME DP - Unbound Medicine ER -