Headspace Gas Chromatographic Determination of Residual 1,3-Butadiene in Rubber-Modified Plastics and Its Migration from Plastic Containers into Selected Foods

1987 ◽  
Vol 70 (1) ◽  
pp. 18-21
Author(s):  
Timothy P Mcneal ◽  
Charles V Breder
Keyword(s):  
Chromatographic Determination ◽  
Chewing Gum ◽  
Flame Ionization ◽  
External Calibration Curve ◽  
Headspace Gas ◽  
The Matrix ◽  
Chromatographic Procedure ◽  
Standard Additions ◽  
Plastic Containers

Abstract A headspace gas chromatographic procedure has been developed for the determination of 1,3-butadiene in rubber-modified plastics and in some foods. Polymer solutions or foods are equilibrated in sealed vials at 90°C, and headspace samples are injected into a gas chromatograph. 1,3-Butadiene residues are measured using a flame ionization detector and are quantitated by the method of standard additions or an external calibration curve. Refrigerator tubs, vegetable oil bottles, chewing gum, and foods in contact with this type of packaging were analyzed. Limits of quantitation varied with the matrix, ranging from 2 ng/g (ppb) in chewing gum to 20 ng/g in polymers. 1,3-Butadiene was found in one polymer at 53 ng/g with an 8% coefficient of variation. The procedure yields "apparent" trace levels of 1,3-butadiene, and confirmation by a complementary technique is required.

Improved Cleanup and Derivatization for Gas Chromatographic Determination of Monosodium Glutamate in Foods

1983 ◽  
Vol 66 (6) ◽  
pp. 1528-1531 ◽  
Author(s):  
Hiroshi Nakanishi
Keyword(s):  
Glutamic Acid ◽  
Acid Derivative ◽  
Monosodium Glutamate ◽  
Chromatographic Determination ◽  
Flame Ionization Detection ◽  
Gas Chromatograph ◽  
Flame Ionization ◽  
Acetone Water ◽  
Chromatographic Procedure

Abstract A gas chromatographic procedure is described for determining monosodium glutamate (MSG) in several types of food. A sample is extracted with acetone- water (1 + 1). Acetone is evaporated and an aliquot of the extract is buffered with 1M NH4OH-1M NH4CI pH 9 solution, and chromatographed directly on a column of QAE Sephadex A-25 that has been pretreated with the same buffer. MSG is eluted with 0.1N HC1, and a portion of the eluate is evaporated to dryness and reacted with dimethylformamide( DMF)-dimethylacetal to form the glutamic acid derivative, which is injected into a gas chromatograph and measured by flame ionization detection. Recoveries of MSG from sample fortified at 5-500 mg ranged from 92.8 to 100%.

scholarly journals Headspace Gas Chromatographic Determination of 1,3-Butadiene in Simulated Saliva

2000 ◽  
Vol 83 (4) ◽  
pp. 929-932 ◽  
Author(s):  
Shirley Abrantes ◽  
Tereza C Dos Santos ◽  
Grazieli SimÕES
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Calibration Graph ◽  
Chewing Gum ◽  
Preliminary Assessment ◽  
Headspace Gas ◽  
Sensitive Determination ◽  
Headspace Gc ◽  
Migration Limit

Abstract A headspace gas chromatographic (GC) method was developed to determine 1,3-butadiene (1,3-BD) in simulated saliva in contact with chewing gum. The calibration graph was linear, and the limit of detection was 0.004 mg/L, which is well below the migration limit for this substance. The headspace GC method provides rapid and reliable analysis for monitoring 1,3-BD migration from chewing gum into simulated saliva. In this paper, we report headspace methodology for sensitive determination of 1,3-BD in chewing gum and results of selected analyses, enabling preliminary assessment of possible exposure to 1,3-BD through migration.

Gas Chromatographic Determination of 1,4-Dioxane in Polysorbate 60 and Polysorbate 80

1979 ◽  
Vol 62 (4) ◽  
pp. 931-936
Author(s):  
Thomas J Birkel ◽  
Charles R Warner ◽  
Thomas Fazio
Keyword(s):  
Quantitative Determination ◽  
Vacuum Distillation ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Polysorbate 80 ◽  
Flame Ionization ◽  
The Matrix ◽  
Carrier Solvent ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is presented for the quantitative determination of 1,4- dioxane in polysorbate 60 and polysorbate 80. Dioxane is isolated from the matrix by closedsystem vacuum distillation with water as the carrier solvent. The distillate is chromatographed on Chromosorb 104 and detected by flame ionization. Recoveries of dioxane from polysorbate 60 samples fortified at 0.5, 1, 2, and 20 ppm averaged 90, 91, 85, and 75%, respectively. Recoveries from polysorbate 80 fortified at the same levels averaged 100, 88, 95, and 95%, respectively. Samples of polysorbate 60 and polysorbate 80 were found to contain from 5.5 to 378 ppm dioxane.

Headspace Gas Chromatographic Determination of Methylene Chloride in Decaffeinated Tea and Coffee, with Electrolytic Conductivity Detection

1984 ◽  
Vol 67 (4) ◽  
pp. 757-761
Author(s):  
B Denis Page ◽  
Claudette F Charbonneau
Keyword(s):  
Methylene Chloride ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Electrolytic Conductivity ◽  
Aqueous Sodium ◽  
Coefficients Of Variation ◽  
Headspace Gas ◽  
Chromatographic Procedure ◽  
Sample Homogeneity

Abstract A headspace gas chromatographic procedure is described for the determination of methylene chloride (MC) in decaffeinated tea and coffee. The tea or coffee sample, with added methylene bromide (MB) internal standard, is equilibrated for 1.5 h at 100°C in aqueous sodium sulfate before manual headspace sampling. MC and MB are separated on a Porasil A column at 160°C and detected by using a Coulson electrolytic conductivity detector. For coffee and tea samples spiked at 1.3 ppm MC, as well as commercially decaffeinated teas and coffees containing up to 8 ppm MC, coefficients of variation were 10% or less. For decaffeinated teas, problems involving sample homogeneity and loss of MC before sealing the headspace vial had to be overcome. Similar problems with decaffeinated instant and ground coffees were minimal. The headspace procedure was superior to a previously reported distillation technique. MC was readily detected at 0.05 ppm. Fourteen decaffeinated teas and 15 decaffeinated coffees were analyzed; MC was detected at levels that ranged up to 15.9 and 4.0 ppm, respectively.

Gas-Liquid Chromatographic Determination of Chlorpyriphos in Dursban Insecticide Formulations

1973 ◽  
Vol 56 (5) ◽  
pp. 1093-1095
Author(s):  
Alan R Hanks ◽  
Barbara S Engdahl ◽  
Billy M Colvin
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Good Precision ◽  
Total Chloride ◽  
Flame Ionization ◽  
Sample Extract ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic method, using flame ionization detection and a column packed with OV-17/QF-1 on Gas-Chrom Q, is described. Chlorpyriphos is extracted from the formulation with chloroform, and dieldrin is added as an internal standard. The sample extract is injected into a gas chromatograph, and peak height ratios are used for quantitative measurement. Applicacation of the method to commercial samples gives good precision. The gas chromatographic procedure is far superior to the total chloride method for the determination of chlorpyriphos and yields values in close agreement to those obtained by infrared and colorimetric methods.

Quantitative Multiresidue Analyses for Volatile Organics in Water and Milk, Using a Fused Silica Open-Tubular Wide-Bore Capillary Column and Automated Headspace Gas Chromatography

1990 ◽  
Vol 73 (2) ◽  
pp. 328-331
Author(s):  
Timothy P Mcneal ◽  
Henry C Hollifield
Keyword(s):  
Gas Chromatography ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Capillary Columns ◽  
Fused Silica ◽  
Headspace Gas Chromatography ◽  
Flame Ionization ◽  
Headspace Gas ◽  
Standard Additions

Abstract A modified multiresidue capillary gas chromatographic (GC) procedure has been developed using automated headspace sampling and a wide-bore fused silica open-tubular (FSOT) capillary column for the determination of volatiles in water and milk. Compounds are quantltated by the method of standard additions. An IBM System 9000 computer with the CAPMC3 chromatographic applications package and a BASIC linear regression program are used for data reduction. Data are presented for solutions prepared by fortifying water and milk with volatile solvents such as acetone, methyl ethyl ketone, benzene, methylene chloride, and chloroform, which are commonly used in the manufacture of packaging materials and adheslves. The wide-bore FSOT capillary columns showed dramatically improved detection for certain compounds, compared with normal-bore capillary GC columns. Data presented for various chemicals demonstrate the improved limits of detection from the use of automated headspace gas chromatography with wide-bore capillary columns and flame ionization detection.

Gas-Liquid Chromatographic Determination of Residues of Methane sulfonate of m-Aminobenzoic Acid Ethyl Ester in Fish

1977 ◽  
Vol 60 (4) ◽  
pp. 961-962
Author(s):  
Joe B Sills ◽  
Charles W Luhning
Keyword(s):  
Ethyl Ester ◽  
Acid Ethyl Ester ◽  
Chromatographic Determination ◽  
Fish Muscle ◽  
Aminobenzoic Acid ◽  
Flame Ionization ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract In this gas-liquid chromatographic procedure for determining residues of methanesulfonate of m-aminobenzoic acid ethyl ester (MS-222) in fish muscle, homogenized tissue is extracted with distilled water, and proteins are removed by coagulation with trichloroacetic acid, centrifugation, and filtration. After careful pH adjustment of the filtrate, MS-222 is partitioned into benzene-ethyl ether and measured by alkali flame ionization gas chromatography. Tissues with known additions of 1–19 μg MS-222/ g were analyzed, with recoveries of 84–95%.

Gas-Liquid Chromatographic Determination of Strychnine in Grain Baits

1975 ◽  
Vol 58 (5) ◽  
pp. 961-964 ◽  
Author(s):  
Alan R Hanks ◽  
Barbara S Engdahl ◽  
Billy M Colvin
Keyword(s):  
Internal Standard ◽  
Chromatographic Determination ◽  
Peak Height ◽  
Good Precision ◽  
Flame Ionization ◽  
Glass Column ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic procedure, using a 6’ × ¼“ glass column packed with 5% SE-30 on Chromosorb W (DMCS) and a flame ionization detector, is described. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform containing an internal standard, 1,3,5-triphenylbenzene. Without further cleanup, extract nitrates are injected directly into a gas chromatograph. Peak height ratios are used for quantitation of strychnine. The analysis of commercial samples shows that the method compares well with a commonly employed ultraviolet spectrophotometric method; good precision, with recoveries ranging from 89.9 to 91.7%, is obtained in the analysis of prepared samples. The method is sensitive to 2 μg strychnine.

Gas Chromatographic Method for Determination of Dimethylamine, Trimethylamine, and Trimethylamine Oxide in Fish-Meat Frankfurters

1991 ◽  
Vol 74 (2) ◽  
pp. 400-403
Author(s):  
Walter Fiddler ◽  
Robert C Doerr ◽  
Robert A Gates
Keyword(s):  
Atlantic Menhaden ◽  
Chromatographic Technique ◽  
Acid Extraction ◽  
Fish Meat ◽  
Flame Ionization ◽  
Trimethylamine Oxide ◽  
Headspace Gas ◽  
Gas Chromatographic Method ◽  
Gas Tight

Abstract A method Is described for analysis of minced fish-meat and surlmi-meat frankfurters for dimethylamine (DMA), trimethyiamine (TMA), and trimethyiamine oxide (TMAO) using a headspace-gas chromatographic technique. After simple acid extraction and addition of NaOH, the headspace was directly Injected Into a gas chromatograph by a gas-tight syringe. DMA and TMA were separated on a Chromosorb 103 column and detected by a flame Ionization detector. TMAO was measured as TMA after Zn reduction. Repeatability of the method for DMA, TMA, and TMAO was 6.6,1.0, and 18.8 ppm, respectively. The method was applicable to Alaska pollock-meat and Atlantic menhaden-meat frankfurters, unwashed, and washed mince and surlml.

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