Fast Analytical Methodology Based on Mass Spectrometry for the Determination of Volatile Biomarkers in Saliva

2011 ◽  
Vol 84 (1) ◽  
pp. 379-385 ◽  
Author(s):  
Miguel del Nogal Sánchez ◽  
Elena Hernández García ◽  
José Luis Pérez Pavón ◽  
Bernardo Moreno Cordero
2005 ◽  
Vol 88 (6) ◽  
pp. 1834-1839 ◽  
Author(s):  
Nicholas G Tsiropoulos ◽  
Konstantinos Liapis ◽  
Dimitrios T Likas ◽  
George E Miliadis

Abstract Analytical methodology was developed and validated for the determination of spiroxamine residues in grapes, must, and wine by gas chromatography/ion trap-mass spectrometry (GC/IT-MS). Two extraction procedures were used: the first involved grapes, must, and wine extraction with alkaline cyclohexane–dichloromethane (9 + 1, v/v) solution, and the second grape extraction with acetone, dichloromethane, and petroleum ether. In both procedures, the extract was centrifuged, evaporated to dryness, and reconstituted in cyclohexane or 2,2,4-trimethylpentane–toluene (9 + 1, v/v), respectively. Spiroxamine diastereomers A and B were determined by GC/IT-MS, and a matrix effect was observed in the case of grapes but not in must and wine. Recovery of spiroxamine from fortified samples at 0.02 to 5.0 mg/kg ranged from 78–102% for grapes and must, with relative standard deviation (RSD) <13%; for red and white wines, recoveries ranged from 90 to 101% with RSD <9%. The limit of quantification was 0.02 mg/kg for grapes, must, and wine or 0.10 mg/kg for grapes, depending on the extraction procedure used.


2016 ◽  
Vol 31 (7) ◽  
pp. 1480-1489 ◽  
Author(s):  
Abhijit Saha ◽  
Sadhan Bijoy Deb ◽  
Manoj Kumar Saxena

Development of a common analytical methodology for the determination of trace impurities in U–Ti, U–Zr and U–Mo alloy fuels by inductively coupled plasma mass spectrometry.


2015 ◽  
Vol 7 (22) ◽  
pp. 9504-9512 ◽  
Author(s):  
Eduardo de Gerónimo ◽  
Ana María Botero-Coy ◽  
José M. Marín ◽  
Virginia C. Aparicio ◽  
José L. Costa ◽  
...  

A multi-residue determination of pesticides in soils using LC-MS/MS has been developed.


Author(s):  
Diana Mariño ◽  
Nancy Patiño

Abstract The presence and use of carbamate and organophosphate pesticides with agricultural and urban purposes in Colombia has been justified for pest control. However, these substances pose a national problem because of their toxic nature, which is associated with accidental poisoning or even with homicides or suicides related to acute fatal poisoning. This study aims to develop and to validate an analytical methodology for the determination of the aldicarb, carbofuran and methamidophos pesticides in blood through liquid chromatography tandem mass spectrometry (LC–MS-MS). To this end, the method for extracting pesticides from the blood was developed, the conditions of LC were defined, the instrumental system MS-MS was optimized and the bioanalytical methodology was validated. This methodology proved to be selective, precise, accurate and linear in the concentration range from 0.10 to 5.0 µg/mL, with a limit of detection of 0.020 µg/mL for aldicarb and carbofuran and 0.050 µg/mL for methamidophos, recovery between 90% and 102%, and stability at room temperature and in the autosampler between 80% and 120%. The analytical methodology was applied to 34 forensic cases. Carbofuran was found at a concentration ranging from 0.020 to >5.0 µg/mL, aldicarb was found at a concentration ranging from 0.10 to 2.5 µg/mL and methamidophos was found at a concentration >5.0 µg/mL. In 62% of the cases, the pesticides under study were used to commit suicide. Necropsy findings of pesticide poisoning are non-specific. Therefore, toxicological blood analysis provides significant information at the forensic level, and the analytical method validated represents a sensitive, fast and reliable analysis with little solvent consumption of a small sample amount, so it is suitable for routine application in fatal pesticide poisonings.


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