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Determination of cephalomannine in rat plasma by gradient elution UPLC-MS/MS method.

Abstract

A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed and validated for the determination and pharmacokinetic investigation of cephalomannine in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2 mL of perchloric acid-methanol (1:9, v/v) to a 0.1 mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile-0.1% formic acid in water with gradient elution. The total run time was 2.0 min and the elution of cephalomannine was at 1.60 min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring (MRM) mode using the respective transitions m/z 832.8→264.1 for cephalomannine and m/z 812.6→286.0 for 10-DAT (internal standard), respectively. The calibration curve was linear over the range of 10-2,000 ng/mL with a lower limit of quantitation (LLOQ) of 10 ng/mL. Mean recovery of cephalomannine in plasma was in the range of 80.9-85.3%. Intra-day and inter-day precision were both <11.2%. This method was successfully applied in pharmacokinetic study after intravenous administration of 5.0mg/kg cephalomannine in rats.

Authors+Show Affiliations

Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Medical College of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Medical College of Henan University of Science and Technology, Luoyang, Henan 471003, PR China.Department of Oncology, Cancer Institute, The First Affiliated Hospital of Henan University of Science and Technology, Luoyang, Henan 471003, PR China. Electronic address: gsg112258@163.com.

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

24929960

Citation

Wang, Xin-Shuai, et al. "Determination of Cephalomannine in Rat Plasma By Gradient Elution UPLC-MS/MS Method." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 963, 2014, pp. 70-4.
Wang XS, Sun JC, Yang RN, et al. Determination of cephalomannine in rat plasma by gradient elution UPLC-MS/MS method. J Chromatogr B Analyt Technol Biomed Life Sci. 2014;963:70-4.
Wang, X. S., Sun, J. C., Yang, R. N., Ren, J., Liang, S., Sun, M., Wang, Y. F., & Gao, S. G. (2014). Determination of cephalomannine in rat plasma by gradient elution UPLC-MS/MS method. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 963, 70-4. https://doi.org/10.1016/j.jchromb.2014.05.045
Wang XS, et al. Determination of Cephalomannine in Rat Plasma By Gradient Elution UPLC-MS/MS Method. J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jul 15;963:70-4. PubMed PMID: 24929960.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of cephalomannine in rat plasma by gradient elution UPLC-MS/MS method. AU - Wang,Xin-Shuai, AU - Sun,Jia-Chun, AU - Yang,Rui-Na, AU - Ren,Jing, AU - Liang,Shuo, AU - Sun,Ming, AU - Wang,Ying-Fei, AU - Gao,She-Gan, Y1 - 2014/06/02/ PY - 2014/02/06/received PY - 2014/05/19/revised PY - 2014/05/25/accepted PY - 2014/6/16/entrez PY - 2014/6/16/pubmed PY - 2015/2/13/medline KW - Cephalomannine KW - Pharmacokinetics KW - Rat plasma KW - UPLC–MS/MS SP - 70 EP - 4 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 963 N2 - A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed and validated for the determination and pharmacokinetic investigation of cephalomannine in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2 mL of perchloric acid-methanol (1:9, v/v) to a 0.1 mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile-0.1% formic acid in water with gradient elution. The total run time was 2.0 min and the elution of cephalomannine was at 1.60 min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring (MRM) mode using the respective transitions m/z 832.8→264.1 for cephalomannine and m/z 812.6→286.0 for 10-DAT (internal standard), respectively. The calibration curve was linear over the range of 10-2,000 ng/mL with a lower limit of quantitation (LLOQ) of 10 ng/mL. Mean recovery of cephalomannine in plasma was in the range of 80.9-85.3%. Intra-day and inter-day precision were both <11.2%. This method was successfully applied in pharmacokinetic study after intravenous administration of 5.0mg/kg cephalomannine in rats. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/24929960/Determination_of_cephalomannine_in_rat_plasma_by_gradient_elution_UPLC_MS/MS_method_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(14)00360-2 DB - PRIME DP - Unbound Medicine ER -