Gas Chromatographic/Mass Spectrometric Determination of α-Methylstyrene in Styrene-Based Polymers and Food Simulants

1991 ◽  
Vol 74 (5) ◽  
pp. 815-818
Author(s):  
Shigeru Tan ◽  
Takashi Tatsuno ◽  
Taro Okada

Abstract A selected ion monitoring method is described for the analysis of styrene (St)-based polymers for a-methylstyrene (α- MSt) and for determining the level of α-MSt migration from St-based sheets Into 4 food simulants. The polymers are dissolved in dlchloromethane; α-MSt Is determined by direct Injection of the polymer solutions. α-MSt migration from St-based sheet to water, 4% acetic acid, 20% ethanol, and n-heptane was measured by gas chromatography/mass spectrometry, using multiple ion monitoring of Ions at mix 118,78, and 91. α-MSt can be quantltated at levels as low as 10 μ/g in the polymer and 0.01 μ/g In the food simulants. Recoveries were 83-113% from St-based sheets and 90-99% from food simulants, respectively.

1993 ◽  
Vol 76 (4) ◽  
pp. 760-764 ◽  
Author(s):  
Sue M Jickells ◽  
Mark R Philo ◽  
John Gilbert ◽  
Laurence Castle

Abstract Benzene in poly(tetrafluoroethylene) (PTFE) coatings of nonstick cookware was determined by heating a small amount of coating in a sealed vial. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the vial headspace for benzene. A small survey (26 samples) of retail nonstick cookware detected benzene ranging from 2 to 50 μg/dm2 in 7 samples. Nonstick frying pans with various polymer coatings were obtained directly from 1 manufacturer. Benzene (6–30 μg/dm2) was detected in a number of these samples and was attributed to the use of a phenylmethyl silicone ingredient that contained benzene at 360 mg/kg. To determine the possible transfer of benzene from these coatings during normal use, several foods (puddings, cakes, and roast potatoes) were prepared in previously unused cookware. The foods were analyzed by using static headspace GC/MS. Benzene was not detected in any of these foods at a limit of detection of 2 μg/kg. In related studies, the determination of benzene release from microwave susceptors was performed by heating the materials in a sealed system at 190PC for 4 min. Benzene release above 1 μg/dm2 was not detected in 24 samples of susceptors. However, 1 specially supplied sample of nonmetallized susceptor released 10 μg/dm2 benzene when heated above normal anticipated temperatures of usage (to 220°C). Foods such as french fries and pizza when cooked according to the manufacturer’s instructions in susceptors contained no benzene with a limit of detection of 2 μg/kg. Even under abuse conditions of susceptors, the transfer of benzene to foods remained below this limit.


1973 ◽  
Vol 19 (9) ◽  
pp. 963-966 ◽  
Author(s):  
Thomas A Witten ◽  
Steven P Levine ◽  
Mary T Killian ◽  
Peter J R Boyle ◽  
Sanford P Markey

Abstract Urinary acid metabolic profiles of 26 healthy young adults who were maintained on a palatable standard diet for three days have been studied by combined gas chromatography-mass spectrometry. Means and standard deviations of the excretion rates of individual, identified acids were determined after the ingestion of ethanol and compared to basal values previously reported. A significant net effect of ethanol was demonstrated for only six of the acids studied: α- and β-hydroxybutyric, adipic, β-methyladipic, p-hydroxyphenylacetic, and 2,5-furandicarboxylic acids.


1994 ◽  
Vol 40 (2) ◽  
pp. 216-220 ◽  
Author(s):  
A H Wu ◽  
D Ostheimer ◽  
M Cremese ◽  
E Forte ◽  
D Hill

Abstract Interference by substances coeluting with targeted drugs is a general problem for gas chromatographic/mass spectrometric analysis of urine. To characterize these interferences, we examined human urine samples containing benzoylecgonine and fluconazole, and other drug combinations including deuterated internal standards that coelute (ISd,c) with target drugs, by selected-ion monitoring (SIM) and full-scan mass spectrometry. We show that, by SIM analysis, detecting the presence of an interferent is dependent on the specific IS used for the assay. When an ISd,c is used, the presence of another coeluting substance (interferent) suggests that the intensity of IS ions is substantially diminished, because the interferent affects both the ISd,c and target drug. When a noncoeluting IS (ISnc) is used, the interferent cannot be discerned unless it coincidently contains one or more of the ions monitored for either the target drug or ISnc. Under full-scan analysis, a coeluting interferent is directly discernable by examining the total ion gas chromatogram.


Processes ◽  
2021 ◽  
Vol 9 (9) ◽  
pp. 1571
Author(s):  
Patricia Jové ◽  
Marina Vives-Mestres ◽  
Raquel De Nadal ◽  
Maria Verdum

Compounds 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA), 2-methylisoborneol (2MIB) and geosmin (GSM) have been reported as being responsible for cork and wine taint. A sustainable method based on thermal desorption-gas chromatography–mass spectrometry (TD-GC/MS) has been developed and optimized, taking into account desorption parameters and chromatographic and mass spectrometric conditions. The combination of parameters that jointly maximized the compound detection was as follows: desorption temperature at 300 °C, desorption time at 30 min, cryo-temperature at 20 °C and trap high temperature at 305 °C. The proposed methodology showed a good linearity (R ≤ 0.994) within the tested range (from 0.1 to 2 ng) for all target compounds. The precision expressed as repeatability and reproducibility was RSD < 10% in both. The limits of quantification ranged from 0.05 to 0.1 ng. The developed methodology and the sampling rates (R-values) of all targeted compounds (from 0.013 to 0.071 m3 h−1) were applied to the air analysis of two wineries. The results showed that the developed methodology is a sustainable and useful tool for the determination of these compounds in air.


1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.


1972 ◽  
Vol 55 (1) ◽  
pp. 85-92 ◽  
Author(s):  
David Firestone ◽  
John Ress ◽  
N L Brown ◽  
R P Barron ◽  
J N Damico

Abstract Twenty-one commercial chlorophenols were examined for the presence of polychlorodibenzo- p-dioxins (chlorodioxins) and related compounds. The chlorophenols were dissolved in aqueous alkali, extracted with petroleum ether, and fractionated on an alumina column. Alumina fractions were examined by electron capture gas chromatography and combined gas chromatography-mass spectrometry. Chlorodioxin content was estimated by electron capture gas chromatography. The presence of chlorodioxins, polychlorodibenzofurans (chlorofurans), and polychlorodiphenyl ethers (chloroethers) was confirmed by combined gas chromatography-mass spectrometry. The 2,3,-7,8-tetrachlorodioxin was found in 3 of 6 samples of 2,4,5-trichlorophenol but was not detected in any of the 11 samples of tetra- and pentachlorophenol that were examined. Hexachlorodioxin was present at levels ranging from 0.17 to 39 ppm in all 8 pentachlorophenols examined. Hexa-, hepta-, and octachlorodioxins as well as a wide variety of chlorofurans and chloroethers of varying chlorine content were present in most of the tetra- and pentachlorophenols. In addition, the gas chromatographic- mass spectrometric data suggested that some of the chlorophenols contained methoxy- and dimethoxypolychlorofurans and methoxypolychloroethers as well as polychlorohy droxybiphenyl.


1990 ◽  
Vol 73 (6) ◽  
pp. 886-892 ◽  
Author(s):  
Keigo Takatsuki ◽  
Tadashi Kikuchi

Abstract A gas chromatographlc-mass spectrometric method using selected Ion monitoring mode for simultaneous determination of 6 sulfonamides in egg and edible animal tissues has been developed. Sulfonamides are extracted from a sample with acetonltrlle. The extract Is passed through a silica cartridge column and concentrated. Dlazomethane in ether Is added to methylate sulfonamides. After evaporation, the residue Is dissolved In methylene chloride and cleaned up by silica gel column chromatography. The methylene chloride eluate containing sulfonamide-methyl derivatives Is evaporated to dryness, redlssolved In ether and partitioned between 6N hydrochloric acid. The acid phase is made alkaline, extracted with ether, and the ether solution, after concentration, Is analyzed by gas chromatography-mass spectrometry in selected Ion monitoring mode. Average recoveries from egg and silver salmon fortified at 1 and 0.2 ppm levels with 6 sulfonamides are 99.2 and 84.3%, respectively; coefficients of variation are 7.03 and 11.20%, respectively. Detection limits are 0.01-0.05 ppm.


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