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Development and validation of liquid chromatography-tandem mass spectrometry method for quantification of a potential anticancer triterpene saponin from seeds of Nigella glandulifera in rat plasma: application to a pharmacokinetic study.

Abstract

Nigella glandulifera Freyn et Sit is a folk medicinal plant, whose seeds show significant anticancer activities attributed to triterpene saponins and volatile oil. In this study, an in vitro cytotoxicity assay demonstrated that Nigella A, the major component of triterpene saponins extracted from N. glandulifera, exhibited growth inhibition in the human lung carcinoma A-549 cell line. Due to this potential activity, a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify Nigella A in rat plasma for a pharmacokinetic study was developed. Nigella A and pravastatin, as internal standard (IS), were extracted from rat plasma using acetonitrile to precipitate protein. Separation was performed on an Agilent Zorbax SB-Aq (3.0 × 150 mm, 3.5 μm) column using a gradient elution method with acetonitrile-0.1% formic acid in water at a flow rate of 0.35 mL/min. Detection was performed using an electrospray ionization in a negative ion multiple reaction monitoring mode. The deprotonated precursor to product ion transitions monitored for Nigella A and IS was at m/z 1352.7→882.6 and m/z 423.1→321.0, respectively. The linear range was 0.240-120 μg/mL with a square regression coefficient (r=0.9996). The intra-day and inter-day precision was less than 6.93%. The simple extraction procedure provided recovery ranged from 92.32 to 95.44% for both analyte and IS. The method was proved to be reliable, precise, and accurate, and was successfully applied to a pharmacokinetic study of Nigella A in rats after i.v. administration via the tail vein at doses of 10, 20, and 30 mg/kg.

Authors+Show Affiliations

Research Center for Clinical Pharmacy, First Affiliated Hospital, Zhejiang University, Hangzhou 310003, PR China.Institute of Clinical Pharmaceutical Research, Hunan Provincial Tumor Hospital/Affiliated Tumor Hospital of Xiangya Medical School of Central South University, Changsha 410013, PR China.Department of Biomedical Engineering, Zhejiang University, Hangzhou 310027, PR China.Department of Biomedical Engineering, Zhejiang University, Hangzhou 310027, PR China.Research Center for Clinical Pharmacy, First Affiliated Hospital, Zhejiang University, Hangzhou 310003, PR China.Research Center for Clinical Pharmacy, First Affiliated Hospital, Zhejiang University, Hangzhou 310003, PR China.Research Center for Clinical Pharmacy, First Affiliated Hospital, Zhejiang University, Hangzhou 310003, PR China. Electronic address: stjz@zju.edu.cn.Department of Biomedical Engineering, Zhejiang University, Hangzhou 310027, PR China. Electronic address: zhanglin@zju.edu.cn.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

25108106

Citation

Hu, Xingjiang, et al. "Development and Validation of Liquid Chromatography-tandem Mass Spectrometry Method for Quantification of a Potential Anticancer Triterpene Saponin From Seeds of Nigella Glandulifera in Rat Plasma: Application to a Pharmacokinetic Study." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 967, 2014, pp. 156-61.
Hu X, Liu X, Gong M, et al. Development and validation of liquid chromatography-tandem mass spectrometry method for quantification of a potential anticancer triterpene saponin from seeds of Nigella glandulifera in rat plasma: application to a pharmacokinetic study. J Chromatogr B Analyt Technol Biomed Life Sci. 2014;967:156-61.
Hu, X., Liu, X., Gong, M., Luan, M., Zheng, Y., Wu, G., Shentu, J., & Zhang, L. (2014). Development and validation of liquid chromatography-tandem mass spectrometry method for quantification of a potential anticancer triterpene saponin from seeds of Nigella glandulifera in rat plasma: application to a pharmacokinetic study. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 967, 156-61. https://doi.org/10.1016/j.jchromb.2014.07.030
Hu X, et al. Development and Validation of Liquid Chromatography-tandem Mass Spectrometry Method for Quantification of a Potential Anticancer Triterpene Saponin From Seeds of Nigella Glandulifera in Rat Plasma: Application to a Pharmacokinetic Study. J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Sep 15;967:156-61. PubMed PMID: 25108106.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Development and validation of liquid chromatography-tandem mass spectrometry method for quantification of a potential anticancer triterpene saponin from seeds of Nigella glandulifera in rat plasma: application to a pharmacokinetic study. AU - Hu,Xingjiang, AU - Liu,Xiaobao, AU - Gong,Minghua, AU - Luan,Ming, AU - Zheng,Yunliang, AU - Wu,Guolan, AU - Shentu,Jianzhong, AU - Zhang,Lin, Y1 - 2014/07/27/ PY - 2014/05/19/received PY - 2014/07/16/revised PY - 2014/07/20/accepted PY - 2014/8/10/entrez PY - 2014/8/12/pubmed PY - 2015/5/12/medline KW - LC–MS/MS KW - Nigella A KW - Pharmacokinetics KW - Rat plasma SP - 156 EP - 61 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 967 N2 - Nigella glandulifera Freyn et Sit is a folk medicinal plant, whose seeds show significant anticancer activities attributed to triterpene saponins and volatile oil. In this study, an in vitro cytotoxicity assay demonstrated that Nigella A, the major component of triterpene saponins extracted from N. glandulifera, exhibited growth inhibition in the human lung carcinoma A-549 cell line. Due to this potential activity, a reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method to quantify Nigella A in rat plasma for a pharmacokinetic study was developed. Nigella A and pravastatin, as internal standard (IS), were extracted from rat plasma using acetonitrile to precipitate protein. Separation was performed on an Agilent Zorbax SB-Aq (3.0 × 150 mm, 3.5 μm) column using a gradient elution method with acetonitrile-0.1% formic acid in water at a flow rate of 0.35 mL/min. Detection was performed using an electrospray ionization in a negative ion multiple reaction monitoring mode. The deprotonated precursor to product ion transitions monitored for Nigella A and IS was at m/z 1352.7→882.6 and m/z 423.1→321.0, respectively. The linear range was 0.240-120 μg/mL with a square regression coefficient (r=0.9996). The intra-day and inter-day precision was less than 6.93%. The simple extraction procedure provided recovery ranged from 92.32 to 95.44% for both analyte and IS. The method was proved to be reliable, precise, and accurate, and was successfully applied to a pharmacokinetic study of Nigella A in rats after i.v. administration via the tail vein at doses of 10, 20, and 30 mg/kg. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/25108106/Development_and_validation_of_liquid_chromatography_tandem_mass_spectrometry_method_for_quantification_of_a_potential_anticancer_triterpene_saponin_from_seeds_of_Nigella_glandulifera_in_rat_plasma:_application_to_a_pharmacokinetic_study_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(14)00495-4 DB - PRIME DP - Unbound Medicine ER -