Simultaneous Quantitative Analysis of Koumine, Gelsemine and Gelsenicine in Biological Samples by LC-MS/MS.
10.3969/j.issn.1004-5619.2017.02.007
- Author:
Sheng Jie JI
1
;
Wei LIU
2
Author Information
1. Department of Forensic Medicine, School of Basic Medical Sciences, Fudan University, Shanghai 200032, China.
2. Shanghai Key Laboratory of Forensic Medicine, Shanghai Forensic Service Platform, Institute of Forensic Science, Ministry of Justice, PRC, Shanghai 200063, China.
- Publication Type:Journal Article
- Keywords:
biological samples;
forensic toxicology;
gelsemine;
gelsenicine;
koumine;
liquid chromatography-tandem mass spectrometry
- MeSH:
Alkaloids/urine*;
Chromatography, High Pressure Liquid;
Chromatography, Liquid;
Forensic Toxicology;
Formates;
Humans;
Indole Alkaloids/urine*;
Liver;
Reproducibility of Results;
Strychnine;
Tandem Mass Spectrometry
- From:
Journal of Forensic Medicine
2017;33(2):141-147
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVES:To establish a LC-MS/MS method which is accurate and sensitive for determination of koumine, gelsemine, and gelsenicine in biological samples and to verify the method.
METHODS:Strychnine was used as internal standard. Analytes in blood, urine and liver with 1% sodium hydroxide solution were extracted by ethyl acetate. Chromatographic separation was achieved on a ZORBAX SB-C₁₈ column （150 mm×2.1 mm, 5 μm）, and gradient elution was performed with the buffer solution of methanol-20 mmol/L ammonium acetate （including 0.1% formic acid and 5% acetonitrile） as mobile phase. Qualitative and quantitative analysis was performed in the multiple reaction monitoring mode coupled with an electrospray ionization source under positive ion mode（ESI⁺）.
RESULTS:The linearity of koumine, gelsemine and gelsenicine in blood, urine and liver was good within corresponding linear limitation and the correlation coefficients （r）>0.995 0. The limits of detection were 0.1 ng/mL （0.1 ng/g）, 0.1 ng/mL （0.1 ng/g） and 0.01 ng/mL （0.01 ng/g）, respectively. The extraction recovery and accuracy of the alkaloids ranged from 61.9% to 114.6% and 92.4% to 114.3%, respectively. The relative standard deviations of the intra-day and inter-day precisions were not more than 11.0%.
CONCLUSIONS:The method is selective, sensitive and suitable for simultaneous determination of koumine, gelsemine and gelsenicine in body fluids and tissues, which offering technical support for clinical diagnosis and treatment and forensic toxicological analysis of Gelsemium elegans poisoning.
