Rapid Determination of Tetrodotoxin in Human Urine and Plasma Using Hydrophilic Interaction Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry
- VernacularTitle:亲水液相色谱三重四极杆质谱联用法快速检测尿液和血浆中河豚毒素
- Author:
Xiuyao ZHANG
;
Xinxin CAI
- Publication Type:Journal Article
- Keywords:
Hydrophilic interaction liquid chromatography-tandem mass spectrometry;
tetrodotoxin;
urine;
plasma
- From:
Chinese Journal of Analytical Chemistry
2009;37(12):1829-1833
- CountryChina
- Language:Chinese
-
Abstract:
A rapid method for the detection of tetrodotoxin(TTX) in human plasma and urine was developed by hydrophilic interaction liquid chromatography-tandem mass spectrometry. After a simple protein precipitation step was undertaken, the subsequent analysis of TTX was achieved on a TSK-gel amide-80 column using an ammonium formate-methanol-acetonitrile gradient with a cycle time of 13 min, and detected by positive electrospray ionization tandem mass spectrometry in the MRM mode, and quantified by matrix-match standard solution. It was found that linearity in urine was observed within concentration ranged from 3 μg/L to 500 μg/L, that in plasma 1 μg/L to 200 μg/L and that limits of detection(S/N=3) for urine and plasma were 1 and 0.3 μg/L, respectively. The average recoveries were 96%-108% and 100%-105% for TTX spiked in urine and plasma, respectively, with relative standard deviations of 1.7%-8.6% and 8.9%-16%(n=6). This method was simple, selective and sensitive to detect TTX in urine and plasma for both clinical and forensic purposes.