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.

Comparison of Gas Chromatographic/Mass Spectrometric and Liquid Chromatographic/Mass Spectrometric Methods for Confirmation of Coumaphos and Its Oxygen Analog in Eggs and Milk

1983 ◽  
Vol 66 (6) ◽  
pp. 1358-1364
Author(s):  
Kevin D White ◽  
Zhao Min ◽  
William C Brumley ◽  
Richard T Krause ◽  
James A Sphon
Keyword(s):  
Mass Spectra ◽  
Chemical Ionization ◽  
Negative Ions ◽  
Mass Spectrometric ◽  
Ionization Mass ◽  
Organophosphate Insecticide ◽  
Ion Detection ◽  
Oxygen Analog ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A comparison of a liquid chromatographic (LC)/mass spectrometric (MS) procedure for confirming coumaphos, an organophosphate insecticide, and its oxygen analog in milk and eggs with a capillary gas chromatographic (GO/MS method is presented. For the confirmation of coumaphos and its oxygen analog, multiple ion detection of both positive and negative ions from the chemical ionization mass spectra was used. Samples of milk and eggs fortified with the 2 compounds at the 0.1,0.01, and 0.005 ppm levels were analyzed. The major finding is the relatively greater efficiency of the LC/MS interface compared with the GC/MS capillary injector.

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.

Gas-Liquid Chromatographic-Mass Spectrometric Detection and Identification of Ambergris

1977 ◽  
Vol 60 (1) ◽  
pp. 160-164 ◽  
Author(s):  
Thomas F Governo ◽  
Rocco T Alessandro ◽  
Manfred J Prager
Keyword(s):  
Mass Spectrometric ◽  
Natural State ◽  
Spectrometric Method ◽  
Gas Liquid Chromatography ◽  
Mass Spectrometric Method ◽  
High Concentration ◽  
Flame Ionization ◽  
Detection And Identification ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A gas-liquid chromatographic-mass spectrometric method for the detection and identification of ambergris in its natural state or in perfume preparations is described. Solid samples are extracted; liquid samples are concentrated. Ambrein, a major component of ambergris, is separated by gas-liquid chromatography on an OV-17 capillary column, detected by flame ionization, and identified by mass spectrometry. Sample retention times and mass spectra were compared with those of purified material isolated from reference ambergris samples. Several types of perfume-related samples were tested. This method was satisfactory for samples of high concentration such as ambergris extracts and also for samples of low ambrein concentration typical of perfume formulations.

Gas-Liquid Chromatographic-Mass Spectrometric Determination of α- and β-Naphthylamines in FD&C Red No. 2 (Amaranth)

1979 ◽  
Vol 62 (5) ◽  
pp. 1020-1026
Author(s):  
Bozidar Stavric ◽  
Raymond Klassen ◽  
Walter Miles
Keyword(s):  
Liquid Chromatography ◽  
Mass Spectrometric ◽  
Gas Liquid Chromatography ◽  
Detectable Amount ◽  
Food Grade ◽  
Mass Spectrometric Determination ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A method is described for the simultaneous quantitation of trace amounts of α- (α-NA) and β-naphthylamines (β-NA) with detectability in the 0.1 ppb range and sensitivity of 50 picomoles in certified food grade amaranth (FD&C Red No. 2; C.I. Food Red 9; CI 16185). The amaranth sample is extracted with benzene, and the evaporated residue is derivatized with perfluorooctanoic anhydride. The resulting derivatives are separated by gas-liquid chromatography and identified and quantitated by mass spectrometric monitoring of the m/e at 539.04. The method was used for quantitation of α-NA and β-NA in randomly chosen samples of amaranth. Of 11 samples from different manufacturers, 5 were free of the β-isomer; the remaining samples contained up to 1.2 ppb β-NA. The concentration of α-NA ranged from no detectable amount to 970 ppb; the majority of the samples contained less than 7 ppb.

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