RESUMO
Objective To investigate a poisoning caused by wild mushrooms and to identify the toxin in these mushrooms.Methods Epidemiological investigation,blood test and mushroom toxin were analyzed.Results This incident was taken place in one family,and all family members were dead.Multiple organ damage was observed in all patients;amatoxins and virotoxins were detected in both mushrooms and the soup,but were not detected in blood samples because of dialysis.Conclusion The incident was caused by wild mushrooms and public education shoud be strenthened to urge people to avoid eating wild mushrooms and go to the hospital immediately if poisoning takes place.
RESUMO
Anultra-performancehydrophilicinteractionliquidchromatography-triplequadrupolemass spectrometric ( UPLC-MS/MS) method was developed for the determination of tetrodotoxin ( TTX) in human urine and plasma. After the sample was cleaned-up and concentrated by immunoaffinity column, the separation of the TTX was carried out on an Acquity UPLC BEH amide column (100 mm×2. 1 mm, 1. 7 μm) with gradient elution using mobile phases of 0. 1% ( V/V) formic acid in water and acetonitrile. The analyte was detected by positive electrospray ionization mass spectrometry in the multiple reaction monitoring ( MRM) mode, and quantified by external solvent standard calibration. The measuring ranges of TTX in urine and plasma were 0. 05-400 μg/L. The average recoveries were 92%-95% and 91%-96% for TTX respectively spiked in urine and plasma with relative standard deviations of 3 . 3%-7 . 2% and 3 . 9%-7 . 8% ( n=5 ) . The limits of detection (LOD, S/N=3) and limits of quantitation (LOQ, S/N=10) of TTX were 0. 02 μg/L and 0. 05μg/L for urine and plasma, respectively. This method is suitable for the detection of TTX in urine and plasma for both forensic and clinical purposes.
RESUMO
A method for the determination of methylmercury ( MeHg ) and ethylmercury ( EtHg ) in aquatic products was developed using gas chromatography-mass spectrometry with stable isotope-labelled internal standard. After ultrasonication assisted hydrochloric acid extraction, MeHg and EtHg in samples were extracted into toluene under the presence of sodium chloride and then back-extracted into cysteine aqueous solution. The MeHg and EtHg were released from their complexes with cysteine by adding cupric ions, and then derived with sodium tetraphenylborate. Under the optimal chromatographic conditions, MeHgPh and EtHgPh, the resulting derivatives, were separated completely on a DB-5MS capillary column and detected by electron impact ionization mass spectrometry in the selective ion monitoring ( SIM) mode, and quantified by a stable isotope dilution method using the d3-methylmercury as internal standard. The calibration curves were linear in the range of 1-500 μg/L of MeHg and EtHg. Concentration of 0. 828 mg Hg/kg with relative standard deviation ( RSD ) of 3 . 2% ( n=6 ) was obtained for MeHg in GBW 10029 . This was in good agreement with the certified values of (0. 84±0. 03) mg Hg/kg. The average recoveries were 94%-101% and 81%-104% for MeHg and EtHg spiked in aquatic samples, with RSDs of 1. 9%-4. 7% and 3. 1%-8. 2%(n=6), respectively. The limits of detection (S/N=3) of the two targets were 0. 1-0. 3μg/kg. This method was sensitive, accurate and could meet the demand of the determination of methylmercury and ethylmercury in aquatic products.
RESUMO
Specific detection of amatoxins and phallotoxins in body fluids is necessary for an early diagnosis of an intoxication with mushrooms.In this study, a rapid method for the simultaneous determination of α-, (β-and γ-amanitin, phalloidin and phallacidin in human urine and plasma was first developed by ultra-perform ance liquid chromatography-tandem mass spectrometry.Urine sample was directly injected into the separation system and plasma sample was initially prepared by precipitation of proteins with 1% acetic acid in acetoni trile.The toxin was analyzed on an ACQUITY UPLC HSS T3 column using a gradient program with a cycle time of 9 min, and detected by positive electrospray ionization tandem mass spectrometry in the MRM mode, and quantified by matrix-match standard solution.The detection limits (S/N = 3) of the toxins were within 0.2-1 μg/L and 0.1-0.5 μg/L for urine and plasma, respectively.The standard curves were linear in the range of 2-100 μg/L for urine and 1-100 μg/L for plasma.The average recoveries were 92.0%-108.0% and 85.0%-100.0% for the toxins spiked in urine and plasma, with RSDs of 1.0%-22.0% and 2.0%-22.0% (n = 6), respectively.The method was simple, selective and sensitive to detect the amatoxins and phallotoxins in urine and plasma for both clinical and forensic purposes.
RESUMO
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.