Fast determination of aconitine in biological materials by LC-MS/MS
10.13618/j.issn.1001-5728.2017.04.015
- VernacularTitle:生物检材中乌头碱的LC-MS/MS快速分析
- Author:
Enyu XU
1
;
Huiya YUAN
;
Lina GAO
;
Junting LIU
Author Information
1. 中国医科大学法医学院法医毒物分析教研室
- Keywords:
forensic toxicological analysis;
biological samples;
HPLC-MS/MS;
aconitum alkaloids;
natural drugs
- From:
Chinese Journal of Forensic Medicine
2017;32(4):393-396
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a HPLC-MS method for determination of aconitum alkaloids in biological samples. Methods The aconitum alkaloids were extracted from the whole blood by using acetonitrile-methanol (5:1 v/v) and then analyzed using HPLC-MS in multiple reaction monitoring (MRM) mode with positive ionization. The analytical column was Agilent Zorbax SB C18 (2.1mm×50mm, 1.8μm)and the mobile phase were water containing 0. 1 % formic acid : acetonitrile (60 : 40 v/v) in isocratic elution. Results The retention time of detection of the aconitine, hypaconitine and mesaconitine were 0.73 min, 0.77 min and 0.63 min, and the precursor product ion combinations of m/z 646.4 → 586.4, 616.1 → 556.5 and 632.4 → 572.1 were used for quantitative analysis, respectively. Calibration curve was linear within the range of 0.1-250 ng/mL with the LOD was 0.1ng/mL, and the coefficient of variation (CV) less than 5.42 % (n=6). The extraction recoveries of aconitine in blood were more than 90 %.Conclusion The results demonstrated that the present method was reliable and robust for natural drugs.
