1.Concentration and determination of strychnine alkaloid in biological fluids.
Jing ZHANG ; Lang-chong HE ; Qiang FU
Journal of Forensic Medicine 2005;21(1):36-38
OBJECTIVE:
To establish a new method for determination of strychnine alkaloid in biological fluids based on molecularly imprinted polymers.
METHODS:
A strychnine molecularly imprinted monolithic column was prepared by in-situ molecularly imprinted technique. The polymer was filled to a 1cm column, and a method was developed to concentrate and determine strychnine alkaloids in biological fluids.
RESULTS:
the limit of detection of the method was 4.9 ng, and the recoveries were more than 92%. The relative standard deviations were smaller than 6.59%. The linear correlation coefficients of standard curves were 0.999 1 and 0.9966 respectively. This method was applied to concentrate and determine strychnine in plasma and urine of poisoned rabbit.
CONCLUSION
The new method could concentrate and simultaneously determine strychnine alkaloids in biological fluids, and it was applied to forensic toxicological analysis.
Alkaloids/analysis*
;
Animals
;
Chromatography, High Pressure Liquid/methods*
;
Humans
;
Male
;
Polymers/chemistry*
;
Rabbits
;
Sensitivity and Specificity
;
Strychnine/urine*
2.Simultaneous Quantitative Analysis of Koumine, Gelsemine and Gelsenicine in Biological Samples by LC-MS/MS.
Journal of Forensic Medicine 2017;33(2):141-147
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.
Alkaloids/urine*
;
Chromatography, High Pressure Liquid
;
Chromatography, Liquid
;
Forensic Toxicology
;
Formates
;
Humans
;
Indole Alkaloids/urine*
;
Liver
;
Reproducibility of Results
;
Strychnine
;
Tandem Mass Spectrometry