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Simultaneous determination of imperatorin and its metabolite xanthotoxol in rat plasma and urine by LC-MS/MS and its application to pharmacokinetic studies.

Abstract

An accurate, precise, selective, and sensitive liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of imperatorin (IMP) and its metabolite, xanthotoxol (XAN), in rat plasma and urine samples. The analytes, along with psoralen as an internal standard, were determined by multiple reaction monitoring (MRM) operated in the positive electrospray ionization (ESI) mode. Chromatographic separation was performed on an Acquity UPLC BEH C18 column (50mm×2.1mm, 1.7μm) with a mobile phase consisting of 0.1% formic acid solution and 0.1% formic acid in methanol at a flow rate of 0.3mL/min. The run time was 6min per sample and the injection volume was 5μL. The method had a lower limit of quantification (LLOQ) of 0.25ng/mL for IMP in plasma and urine, and 1ng/mL for XAN in urine. The linear calibration curves were fitted over the range of 0.25-1000ng/mL for IMP in plasma, 0.25-1000ng/mL for IMP in urine, and 1-1000ng/mL for XAN in urine, with correlation coefficients greater than 0.995. The inter- and intra-day accuracies (relative error, RE%) were between -8.5% and 3.5%, and the precisions (relative standard deviation, RSD%) were less than 10.0% for all quality control samples (QCs). The analytes were extracted from rat plasma and urine samples using a liquid-liquid extraction method with the extraction recovery in the range of 60.3-79.1%. A good stability of the analytes was observed in all the analysis procedures. The method was successfully validated and applied to determine the pharmacokinetics of IMP in rat plasma and, for the first time, the metabolite kinetics of IMP to XAN in rat urine after IMP administration.

Authors+Show Affiliations

College of Pharmacy, Chonnam National University, 77, Yongbong-ro, Buk-gu, Gwangju, 61186, Republic of Korea.College of Pharmacy, Chonnam National University, 77, Yongbong-ro, Buk-gu, Gwangju, 61186, Republic of Korea.Division of Traditional Korean Medicine Resource, National Development Institute of Korean Medicine, 288, Woodland-gil, Anyang-myun, Jangheung, Jeonnam, 59338, Republic of Korea.Division of Traditional Korean Medicine Resource, National Development Institute of Korean Medicine, 288, Woodland-gil, Anyang-myun, Jangheung, Jeonnam, 59338, Republic of Korea.College of Pharmacy, CHA University, 335, Pangyo-ro, Bungdang-gu, Seongnam-si, Gyeonggi-do, 13488, Republic of Korea. Electronic address: hycho@cha.ac.kr.College of Pharmacy, Chonnam National University, 77, Yongbong-ro, Buk-gu, Gwangju, 61186, Republic of Korea. Electronic address: leeyb@chonnam.ac.kr.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

28064067

Citation

Ngo, Lien, et al. "Simultaneous Determination of Imperatorin and Its Metabolite Xanthotoxol in Rat Plasma and Urine By LC-MS/MS and Its Application to Pharmacokinetic Studies." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1044-1045, 2017, pp. 30-38.
Ngo L, Tran P, Ham SH, et al. Simultaneous determination of imperatorin and its metabolite xanthotoxol in rat plasma and urine by LC-MS/MS and its application to pharmacokinetic studies. J Chromatogr B Analyt Technol Biomed Life Sci. 2017;1044-1045:30-38.
Ngo, L., Tran, P., Ham, S. H., Cho, J. H., Cho, H. Y., & Lee, Y. B. (2017). Simultaneous determination of imperatorin and its metabolite xanthotoxol in rat plasma and urine by LC-MS/MS and its application to pharmacokinetic studies. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1044-1045, pp. 30-38. doi:10.1016/j.jchromb.2016.12.037.
Ngo L, et al. Simultaneous Determination of Imperatorin and Its Metabolite Xanthotoxol in Rat Plasma and Urine By LC-MS/MS and Its Application to Pharmacokinetic Studies. J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Feb 15;1044-1045:30-38. PubMed PMID: 28064067.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous determination of imperatorin and its metabolite xanthotoxol in rat plasma and urine by LC-MS/MS and its application to pharmacokinetic studies. AU - Ngo,Lien, AU - Tran,Phuong, AU - Ham,Seong-Ho, AU - Cho,Jung-Hee, AU - Cho,Hea-Young, AU - Lee,Yong-Bok, Y1 - 2016/12/28/ PY - 2016/07/29/received PY - 2016/10/28/revised PY - 2016/12/21/accepted PY - 2017/1/9/pubmed PY - 2017/3/25/medline PY - 2017/1/9/entrez KW - Imperatorin KW - LC–MS/MS KW - Metabolite KW - Pharmacokinetics KW - Xanthotoxol SP - 30 EP - 38 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 1044-1045 N2 - An accurate, precise, selective, and sensitive liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of imperatorin (IMP) and its metabolite, xanthotoxol (XAN), in rat plasma and urine samples. The analytes, along with psoralen as an internal standard, were determined by multiple reaction monitoring (MRM) operated in the positive electrospray ionization (ESI) mode. Chromatographic separation was performed on an Acquity UPLC BEH C18 column (50mm×2.1mm, 1.7μm) with a mobile phase consisting of 0.1% formic acid solution and 0.1% formic acid in methanol at a flow rate of 0.3mL/min. The run time was 6min per sample and the injection volume was 5μL. The method had a lower limit of quantification (LLOQ) of 0.25ng/mL for IMP in plasma and urine, and 1ng/mL for XAN in urine. The linear calibration curves were fitted over the range of 0.25-1000ng/mL for IMP in plasma, 0.25-1000ng/mL for IMP in urine, and 1-1000ng/mL for XAN in urine, with correlation coefficients greater than 0.995. The inter- and intra-day accuracies (relative error, RE%) were between -8.5% and 3.5%, and the precisions (relative standard deviation, RSD%) were less than 10.0% for all quality control samples (QCs). The analytes were extracted from rat plasma and urine samples using a liquid-liquid extraction method with the extraction recovery in the range of 60.3-79.1%. A good stability of the analytes was observed in all the analysis procedures. The method was successfully validated and applied to determine the pharmacokinetics of IMP in rat plasma and, for the first time, the metabolite kinetics of IMP to XAN in rat urine after IMP administration. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/28064067/Simultaneous_determination_of_imperatorin_and_its_metabolite_xanthotoxol_in_rat_plasma_and_urine_by_LC_MS/MS_and_its_application_to_pharmacokinetic_studies_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(16)30547-5 DB - PRIME DP - Unbound Medicine ER -