Gas-Liquid Chromatographic Determination of β-Asarone, A Component of Oil of Calamus, in Flavors and Beverages

1973 ◽  
Vol 56 (5) ◽  
pp. 1281-1283
Author(s):  
Damon Larry

Abstract A method has been developed for the detection and quantitation of β-asarone in vermouths. Volatiles are isolated by steam distillation, and β-asarone is separated from interfering substances by solvent extraction and subjected to gas chromatographic analysis. Quantitation of samples containing 5–100 ppm β-asarone was achieved by direct chromatographic peak comparisons with standards prepared in 20% ethanol-water, which are treated the same as samples. Average recovery from light and dark vermouths spiked at 5, 15, 25, and 100 ppm was 98.8%.

1987 ◽  
Vol 70 (6) ◽  
pp. 1031-1032
Author(s):  
Yuuko S Endoh ◽  
Ryozo Yamaoka ◽  
Nobuo Sasaki

Abstract A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.


1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


1980 ◽  
Vol 63 (1) ◽  
pp. 33-36
Author(s):  
Molly I Keating

Abstract A rapid method for the analysis of dip washes is described which eliminates the usual solvent extraction procedure. The dip wash is initially diluted with acetone and then with petroleum ether. The diluted dip wash is analyzed by gasliquid chromatography, using an alkali ionization detector sensitive to phosphorus compounds. The method was applied to the determination of dioxathion (2,3-ρ-dioxanedithiol S,S-bis(O,O-diethyl phosphorodithioate)), and quintiofos (O-ethyl O-8-quinolyl phenylphosphonothioate) dip washes. Average recoveries from fouled dip washes were 100 and 104%. GLC of these compounds with an internal standard is described, which improves the precision of the method to ±2%.


1983 ◽  
Vol 66 (2) ◽  
pp. 284-286
Author(s):  
Thomas D Macy ◽  
Andrew Loh

Abstract A high pressure liquid chromatographic (HPLC) method has been developed to determine monensin in feed premixes. The method is simple and rapid. Monensin is extracted with methanol-water and determined in the extracting solution by HPLC. Average recovery for monensin from a 13.2% premix sample was 103% (coefficient of variation (CV), 2.6%) by HPLC and compares with the value of 100% (CV, 3.4%) obtained by the turbidimetric bioassay method.


1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.


1979 ◽  
Vol 62 (2) ◽  
pp. 310-314
Author(s):  
Phillip G Vincent ◽  
Beatriz Ferreira Engelke

Abstract A high pressure liquid chromatographic isocratic procedure is described for determining and quantitating the 5 major alkaloids narcotine, papaverine, thebaine, codeine, and morphine in Papaver somniferum L. and thebaine in Papaver bracteatum Lindl. Other papaveraceous alkaloids, including salutaridine, oripavine, laudanosine, isothebaine, cryptopine, alpinigenine, narceine, protopine, and gnoscopine, were also quantitated. The values for morphine, codeine, and thebaine in P. somniferum were in agreement within 5—9% with values obtained by the United Nations Narcotics Laboratory by other methods. In contrast to previously reported procedures, the advantage of this method is that no precolumn or other purification other than solvent extraction of the capsular tissue is necessary. Isocratic chromatography alone on a single column resolved the 5 major alkaloids.


1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.


1982 ◽  
Vol 65 (5) ◽  
pp. 1106-1111
Author(s):  
Terry D Spittler ◽  
Robert J Argauer ◽  
Donald J Lisk ◽  
Ralph O Mumma ◽  
George Winnett ◽  
...  

Abstract Apples from trees treated in the field at 2-week intervals (9 foliar applications) with the synthetic pyrethroid insecticide fenvalerate (cyano(3-phenoxyphenyL)methyl 4-chloro-alpha-(1-methylethyl)- benzeneacetate) were processed into apple sauce, juice, pomace, and peels plus cores. Gas-liquid chromatographic analysis of the commodities for fenvalerate showed the sauce and juice to be essentially residue-free, the whole apples to contain about 0.4 ppm, and the pomace and peels plus cores to contain about 2 and 1.5 ppm, respectively. Agreement among 5 laboratories using modifications of the same basic method was good.


1978 ◽  
Vol 61 (1) ◽  
pp. 08-14 ◽  
Author(s):  
Charles J Stafford ◽  
William L Reichel ◽  
Douglas M Swineford ◽  
Richard M Prouty ◽  
Martha L Gay

Abstract A procedure is described for determining Kepone (decachlorooctahydro-l,3,4-metheno-2H-cyclobuta [cd]pentalene-2-one) residues in avian egg, liver, and tissue. Samples were extracted with benzene-isopropanol, and the extract was cleaned up with fuming H2SO4-concentrated H2SO4. Kepone was separated from organochlorine pesticides and polychlorinated biphenyls on a Florisil column and analyzed by electron capture gas-liquid chromatography GLC). The average recovery from spiked tissues was 86%. The analyses performed on 14 bald eagle carcasses and livers, 3 bald eagle eggs, and 14 osprey eggs show measurable levels which indicate that Kepone accumulates in the tissues of fish-eating birds. Residues were confirmed by GLC-mass spectrometry.


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