Improvedtert-Butyldimethylsilylation Gas Chromatographic/Mass Spectrometric Detection of Nerve Gas Hydrolysis Products from Soils by Pretreatment of Aqueous Alkaline Extraction and Strong Anion-Exchange Solid-Phase Extraction

2002 ◽  
Vol 74 (18) ◽  
pp. 4709-4715 ◽  
Author(s):  
Masaaki Noami ◽  
Mieko Kataoka ◽  
Yasuo Seto
Keyword(s):  
Solid Phase Extraction ◽  
Anion Exchange ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Phase Extraction ◽  
Alkaline Extraction ◽  
Hydrolysis Products ◽  
Strong Anion Exchange ◽  
Chromatographic Mass

Gas Chromatographic/Mass Spectrometric Confirmation of Leucomalachite Green in Catfish (Ictalurus punctatus) Tissue

1995 ◽  
Vol 78 (4) ◽  
pp. 971-977 ◽  
Author(s):  
Sherri B Turnipseed ◽  
José E Roybal ◽  
Jeffrey A Hurlbut ◽  
Austin R Long
Keyword(s):  
Solid Phase Extraction ◽  
Ictalurus Punctatus ◽  
Solid Phase ◽  
Mass Spectrometric ◽  
Phase Extraction ◽  
Neutral Alumina ◽  
Ms Analysis ◽  
Solid Phase Extraction Cartridge ◽  
Leucomalachite Green ◽  
Chromatographic Mass

Abstract A gas chromatographic/mass spectrometric (GC/MS) method was developed to confirm the presence of leucomalachite green (LMG), a metabolite of the triphenylmethane dye malachite green (MG), in catfish tissue. Residues were isolated according to a previously described liquid chromatographic (LC)A/IS spectrometric analysis of MG and LMG in fish. In our isolation procedure, analytes are extracted from tissue with acetonitrile–buffer, partitioned into CH2CI2, and applied to neutral alumina and propylsulfonic acid solid-phase extraction cartridges. Before GC/MS analysis, extracts prepared for the LC determinative method are eluted from a cyano solid-phase extraction cartridge, extracted into organic solvent, and concentrated for GC/MS analysis. Selected ion monitoring was performed by using 5 diagnostic ions (m/z 330,329,253,210, and 165) of LMG. The method was validated by confirming LMG in tissue fortified with mixtures of MG and LMG (5 and 10 ng/g each) and in tissue from fish that had been exposed to low levels of MG.

scholarly journals IDENTIFICATION OF CANNABIMIMETIC MDMB(N)-073F METABOLITES IN URINE BY METHOD OF GAS CHROMATOGRAPHY WITH MASS SPECTROMETRIC DETECTION

2019 ◽  
Vol 7 (2) ◽  
pp. 70-83 ◽  
Author(s):  
S. S. Kataev ◽  
O. N. Dvorskaya ◽  
M. A. Gofenberg
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Acute Poisoning ◽  
Mass Spectrometric ◽  
Mass Spectrometric Detection ◽  
Urine Samples ◽  
Instrumental Method ◽  
Phase Extraction

Background. At the beginning of 2019, the use of a new representative of synthetic cannabimimetics of the methylbutanoate indazole carboxamides group, MDMB(N)-073F, was recorded in a number of regions in the Russian Federation. Characteristic features of the pharmacological effect, the clinical picture of MDMB(N)-073F poisoning have not been studied, the psychoactive effects produced by MDMB(N)-073F remain unexplored. In this regard, the study of the new cannabimimetic metabolism is an important aspect in establishing the fact of taking MDMB(N)-073F during expert studies of biological objects.The aim of the research is identifying metabolites of synthetic MDMB(N)-73F cannabimimetics in real urine samples using solid-phase extraction (SPE) and gas chromatography (GC) with mass spectrometric detection (GC-MS).Materials and methods. 10 urine samples were collected from March 15 to March 29, 2019. 8 urine samples were taken from the medical examination offices of the city of Yekaterinburg and the Sverdlovsk region from the persons examined for intoxication; 2 urine samples were obtained from the patients of the Sverdlovsk regional center of acute poisoning upon enrolment to the toxic-intensive care unit with a preliminary diagnosis of “acute poisoning by synthetic cannabimimetics”. In the research, SampliQ EVIDEX-200 mg – 3 ml (Agilent, USA) cartridges were used for the sample preparation; β-glucuronidase Type HP-2, From Helix Pomatia, 100000 U/ml (Sigma-ALDRICH CHEMI, Germany) was used for enzymatic hydrolysis. Gas chromatography – mass spectrometry with the use of Agilent 7820 gas chromatograph with Agilent 5975 mass selective detector (Agilent, USA) was used as an instrumental method of the analysis.Results. The metabolites that make it possible to establish the fact of taking MDMB(N)-073F cannabimimetics via urine screening procedure to detect the presence of narcotic and medicinal substances with the use of solid-phase extraction and gas chromatography methods with mass spectrometry, have been described. The major metabolites MDMB(N)-073F in the urine of smoking mixtures consumers have been identified. The metabolism of MDMB(N)-073F has been found to be mainly due to hydrolysis of the ester group, hydroxylation, oxidative defluorination and N-dealkylation. Most of the resulting metabolites are excreted in the urine in the conjugated form.Conclusion. Gas chromatographic and mass spectrometric characteristics of some derivatives of the main metabolites of the new synthetic MDMB(N)-073F cannabimimetic have been obtained. This data can be used in the practice of forensic chemical and chemical toxicological analysis.

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