Capillary Gas Chromatographic Determination with Electron Capture Detector of β-Propiolactone in Biological Materials

1991 ◽  
Vol 74 (4) ◽  
pp. 595-599
Author(s):  
Aziz Geahchan ◽  
Bruno Fouillet ◽  
Paul Chambon ◽  
Renee Chambon ◽  
Bahia Nouri
Keyword(s):  
Electron Capture ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Biological Materials ◽  
Electron Capture Detector ◽  
Detector Response ◽  
Limit Of Quantitation ◽  
Low Levels ◽  
Ppm Level

Abstract A method has been developed for the determination of β- propiolactone by derivatizing it to the volatile N-hexyl-3- heptafluorobutanoyloxypropanamide, which can be separated and Identified by a capillary CP-Sil 8 column, and detected by an electron capture detector (ECD). First, β- propiolactone is reacted with N-hexylamine to yield N-hexyl- 3-hydroxypropanamide. The fluorobutanoyl ester derivative is next prepared by using heptafluorobutyrlc acid anhydride in the presence of trimethylamine. The method Is very sensitive, simple, and specific, and can be used to detect and quantitate residual β-propiolactone In Iyophilized biological materials. The limit of detection is 0.2 ppm β-proplolactone in a 50 mg sample; however, because of variability at low levels, the limit of quantitation is 1 ppm. Detector response was linear for 2-500 ng β-propiolactone. Recoveries were 98% or greater from Iyophilized vaccines spiked at the 2-20 ppm level. No side products or interference peaks were observed in the derivatization reaction.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin

1984 ◽  
Vol 67 (2) ◽  
pp. 275-277
Author(s):  
Arnold P Borsetti ◽  
Lee S Thurston
Keyword(s):  
Gas Chromatography ◽  
Liquid Phase ◽  
Electron Capture ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Chromatographic Determination ◽  
Gelatin Matrix ◽  
Limit Of Quantitation ◽  
Acetate Derivative

Abstract A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP-1240DA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Gas Chromatographic Determination of Captan, Folpet, and Captafol Residues in Tomatoes, Cucumbers, and Apples Using a Wide-Bore Capillary Column: Interlaboratory Study

1991 ◽  
Vol 74 (5) ◽  
pp. 830-835 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Capillary Column ◽  
Chromatographic Determination ◽  
Interlaboratory Study ◽  
Electron Capture Detection ◽  
Coefficients Of Variation ◽  
Capillary Column Gas Chromatography ◽  
Ppm Level

Abstract An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multlresidue method modified to Include additional solvent elutlon in the optional Florisll column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol In apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.

Liquid Chromatographic Determination of Benzoyl Peroxide in Acne Preparations

1984 ◽  
Vol 67 (5) ◽  
pp. 913-915
Author(s):  
Chih-Kuang Chou ◽  
David C Locke
Keyword(s):  
Benzoyl Peroxide ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Detector Response ◽  
Electrochemical Detector ◽  
Reverse Phase ◽  
Order Of Magnitude ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid, precise, and accurate liquid chromatographic (LC) method is described for the determination of benzoyl peroxide (BP) in acne preparations. BP is extracted from a water dispersion of the preparation with dichloromethane (DCM), and an aliquot is eluted from a C-18 reverse phase LC column with acetonitrile-O.lOM aqueous NaCI04. Selective and sensitive quantitation is accomplished with a reductive mode electrochemical detector. This detector is an order of magnitude more sensitive than a 240 nm UV absorption detector; the lower limit of detection is 2 ng for a 4 μL injection. The recovery of BP is 99.4% and the detector response is linear to at least 2 μg per 4 μL injection.

Capillary Gas Chromatographic Determination of T-2 Toxin, HT-2 Toxin, and Diacetoxyscirpenol in Cereal Grains

1984 ◽  
Vol 67 (6) ◽  
pp. 1105-1107
Author(s):  
Huguette Cohen ◽  
Michel Lapointe
Keyword(s):  
Electron Capture ◽  
Impact Ionization ◽  
Chromatographic Determination ◽  
Fused Silica ◽  
Electron Capture Detector ◽  
Resolving Power ◽  
Cereal Grains ◽  
Gas Chromatography Mass Spectrometry ◽  
Silica Column

Abstract A capillary gas chromatographic (GC) method using an electron capture detector is described for determining T-2 and HT-2 toxins and diacetoxyscirpenol (DAS) in cereal grains at levels as low as 100 ppb for T-2 and DAS and 50 ppb for HT-2. Samples are extracted with methanol-water according to the Scott method, and further purified on a silica gel cartridge and a cyano column. Heptafluorobutyrylimidazole (HFBI) is added to form the esters of the analytes. Ester(s) of T-2, HT-2 and DAS are separated on a 30 m × 0.32 mm DB-5 fused silica column and measured with a "Ni electron capture detector. Samples were confimed by gas chromatography/mass spectrometry using electron impact ionization and single ion monitoring at the molecular mass of 501.11 m/z for T-2, 665.08 m/z for HT-2, and 502.12 m/z for DAS at 10 000 resolving power. The method was applied to wheat, oats, and barley. Average recoveries ranged from a low of 65% for T- 2 in barley to a high of 99% for DAS in oats.

Liquid Chromatographic Determination of Norflurazon and Its Initial Metabolite in Soil

1994 ◽  
Vol 77 (3) ◽  
pp. 752-755 ◽  
Author(s):  
William T Willian ◽  
Thomas C Mueller
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Detector Response ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Soluble Components

Abstract A rapid, sensitive method for the determination of norflurazon in 4 soils is described. Data on the initial soil metabolite is also obtained in soils with low organic matter. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components by using a C18 column, and fluorescence detection with excitation at 294 nm and emission measured at 398 nm. Recoveries from fortified soils were >90% for norflurazon and >80% for desmethylnorflurazon from the Shipps, Lexington, and Harkey soils. Average percent relative standard deviations over the soils examined was 5.5% for norflurazon and 8.7% for desmethylnorflurazon. The limit of detection for norflurazon was 10 ng/g soil, whereas the limit of detection for desmethylnorflurazon was 100 ng/g soil because of its smaller relative detector response.

scholarly journals Determination of Chloramphenicol Residue in Chicken Tissues by Immunoaffinity Chromatography Cleanup and Gas Chromatography with aMicrocell Electron Capture Detector

2006 ◽  
Vol 89 (2) ◽  
pp. 369-373 ◽  
Author(s):  
Suxia Zhang ◽  
Jinhui Zhou ◽  
Jianzhong Shen ◽  
Shuangyang Ding ◽  
Jiancheng Li
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Chicken Liver ◽  
Electron Capture Detector ◽  
Immunoaffinity Column ◽  
Chicken Tissues ◽  
Chicken Muscle ◽  
Limit Of Quantitation ◽  
Sepharose 4B

Abstract A rapid and sensitive gas chromatography (GC) method was developed to detect chloramphenicol in chicken tissues. The extracted samples were cleaned up using the immunoaffinity column prepared by coupling antichloramphenicol monoclonal antibody with cyanogen bromide-activated Sepharose 4B. The dynamic column capacity of chloramphenicol was 3265 ng/mL gel. The eluate was evaporated to dryness, and residues were derivatized and determined by GC with a microcell electron capture detector. Average recoveries were 86.6 to 96.9 for chicken muscle and 74.3 to 96.1 for chicken liver. The limit of quantitation of the method was 0.05 ng/g for chicken muscle and 0.1 ng/g for chicken liver.

Liquid Chromatographic Determination of 5-(Methylamino)-2-Phenyl-4-[3-(Trifluoromethyl)phenyl]-3-(2H)-Furanone in Soil

1990 ◽  
Vol 73 (2) ◽  
pp. 298-299
Author(s):  
Thomas C Mueller ◽  
Philip A Banks ◽  
Parshall B Bush ◽  
William C Steen
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Soil Types ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A rapid, sensitive method is described for the determination of5-(methylamlno)-2-phenyl-4-[3-(trlfluoromethyl)phenyl]-3- (2M)-furanone (RE-40885) concentrations in 3 soil types. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanolsoluble components using a C18 column, and UV detection at 275 nm. Recoveries were 94, 96, and 94% from the Greenville, Cecil, and Dothan soils, respectively. Average relative standard deviation was 8.0% in the Greenville soil. The qualitative limit of detection was 20 ppb and the limit of quantitation was 40 ppb in 25 g soil samples.

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