Combined Gas-Liquid Chromatographic Mass Spectrometric Analysis of Some Commercial Aryl Phosphate Oils

1978 ◽  
Vol 61 (2) ◽  
pp. 266-271
Author(s):  
Padmakar G Deo ◽  
Philip H Howard
Keyword(s):  
Fire Retardant ◽  
Phosphate Esters ◽  
Spectrometric Analysis ◽  
Gas Liquid Chromatography ◽  
Mass Spectral Data ◽  
Mass Spectral ◽  
Hydraulic Fluids ◽  
Alkyl Phenols ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract Five commercial samples of synthetic aryl phosphate oils, which are widely used as fire retardant hydraulic fluids and as flame retardant plasticizers, have been analyzed by combined gas-liquid chromatography/mass spectrometry (GLC/MS). Each sample contained at least 4 isomers of aryl phosphate esters. The peaks were identified by a close examination of the mass spectral data and, wherever possible, by comparing retention times of the peaks with those of either the purchased or synthesized compounds. One aryl phosphate hydraulic fluid contained a small amount of a hydrocarbon. The results indicate that most of the aryl phosphate esters in the commercial samples were formed from phenol, cresols, xylenols, and other alkyl phenols. No free phenols could be detected in the samples analyzed.

Electron capture gas-liquid chromatographic-mass spectral identification of acids produced by Neisseria meningitidis in a defined medium

1979 ◽  
Vol 9 (1) ◽  
pp. 97-102
Author(s):  
C C Alley ◽  
J B Brooks ◽  
D S Kellogg
Keyword(s):  
Liquid Chromatography ◽  
Neisseria Meningitidis ◽  
Electron Capture ◽  
Defined Medium ◽  
Gas Liquid Chromatography ◽  
Mass Spectral ◽  
Spectral Identification ◽  
Acid Metabolites ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

The acid metabolites and the cellular fatty acids of three strains of Neisseria meningitidis grown in a chemically defined liquid medium were determined with computerized frequency-pulsed electron capture gas-liquid chromatography. Five acids not previously reported were subsequently identified: isobutyric, octanoic, decenoic (C10:1), dodecenoic (C12:1), and tetradecenoic (C14:1). These acids were produced during active metabolism and were not detected as cellular constituents. The frequency-pulsed electron capture gas-liquid chromatography methods which we used provide a rapid, reliable, sensitive means of detecting both these and other metabolic and cellular acids in spent culture medium.

Gas-Liquid Chromatographic-Mass Spectrometric Confirmation of Endosulfan and Endosulfan Sulfate in Apples and Carrots

1981 ◽  
Vol 64 (5) ◽  
pp. 1208-1210
Author(s):  
Perry S Wilkes
Keyword(s):  
Mass Spectra ◽  
Chemical Ionization ◽  
Mass Range ◽  
Mass Spectrometric ◽  
Chromatographic Retention ◽  
Gas Liquid Chromatography ◽  
Endosulfan Sulfate ◽  
Gasliquid Chromatography ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A gas-liquid chromatography-mass spectrometric (GLC-MS) procedure is described for the confirmation of endosulfan I, endosulfan II, and endosulfan sulfate in apples and carrots. After extraction, cleanup, and determination by electron capture gasliquid chromatography using current AOAC methodology, residues are confirmed by GLC-MS. The chemical ionization (CI) mode is used with methane as a reagent gas. Each residue is confirmed by a scan of only 4 regions of its mass spectrum rather than the full mass range. The 4 mass regions for the 2 endosulfan isomers are 274-280, 340-346, 368-374, and 404-412 atomic mass units (amu). For endosulfan sulfate, the mass regions are 286-294, 322-330, 384-392, and 420-428 amu. Four ions and their chlorine isotopic distributions are detected for each compound by this scanning technique. This method was developed by using carrots and apples to which had been added 0.1 ppm (50% of the current legal tolerance on carrots) of each of the 3 pesticides. The gas chromatographic retention times and the mass spectra of the 4 mass regions specified for the 3 pesticides were compared to those of reference standards injected under identical GLC-MS conditions and were used as the basis for confirming identity of the 3 compounds.

Gas Chromatographic and Gas Chromatographic-Mass Spectrometric Confirmation of 2,4- and 2,6-Toluenediamine Determined by Liquid Chromatography in Aqueous Extracts

1982 ◽  
Vol 65 (6) ◽  
pp. 1388-1394 ◽  
Author(s):  
Roger C Snyder ◽  
William C Brumley ◽  
Charles V Breder ◽  
Thomas Fazio
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Mass Spectrometric ◽  
Gas Liquid Chromatography ◽  
Aqueous Extracts ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract The confirmation of 2,4- and 2,6-toluenediamine (TDA) in aqueous extracts from boil-in-bags and retortable pouches is described. The extracts were initially analyzed by a high performance liquid chromatographic procedure and any apparent 2,4- and/or 2,6-TDA were quantitated. The liquid chromatographic effluent corresponding to any apparent 2,4- or 2,6-TDA was collected. TDA was then partitioned into ethyl acetate and reacted with trifluoroacetic anhydride (TFAA). The TDA-TFAA derivative formed was confirmed by gas-liquid chromatography (GLC) using a 1.2 m × 0.32 cm nickel column packed with 6% OV-17 on Superpak-20M. Results obtained from analyzing extracts of several retortable pouches and boil-in-bags showed levels of TDA migration ranging from <0.1 to 2.2 ppb (μg/L). Additional confirmation of the TDA-TFAA derivative from retortable pouches by multiple ion detection GC/mass spectrometry is also described.

Separation and Identification of Neutral and Acidic Metabolites in Cerebrospinal Fluid

1972 ◽  
Vol 18 (3) ◽  
pp. 258-262 ◽  
Author(s):  
L D Waterbury ◽  
L A Pearce
Keyword(s):  
Cerebrospinal Fluid ◽  
Trimethylsilyl Ether ◽  
Gas Liquid Chromatography ◽  
Mass Spectral Data ◽  
Drug Induced ◽  
Mass Spectral ◽  
Human Cerebrospinal Fluid ◽  
Methylene Unit ◽  
Induced Changes ◽  
Potential Use

Abstract We describe a method for obtaining profiles of neutral and acidic substances present in human cerebrospinal fluid (CSF) by gas—liquid chromatography. Metabolites extracted with ethyl acetate and ether are converted to methyl ester, trimethylsilyl ether derivatives. With this technique, acidic metabolites of brain amines, and neutral metabolites of dopamine and norepinephrine have been identified in human CSF. Some of these substances have not been reported previously in CSF. Extracted substances are identified on the basis of their methylene-unit values and mass spectral data. Potential use of this method in neurodiagnosis and in delineating drug-induced changes in CSF metabolites is discussed.

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