Liquid Chromatographic Determination of 2,4-Dinitro-l-Naphthol and 1-Naphthol in External D&C Yellow No. 7

1983 ◽  
Vol 66 (6) ◽  
pp. 1429-1432
Author(s):  
Allen L Goldberg ◽  
Robert J Calvey

Abstract A sensitive, reproducible method that uses liquid chromatography in the reverse phase mode with a C-18 column is described for determining 2,4-dinitro- 1-naphthol and 1-naphthol in Ext. D&C Yellow No. 7. With this method, these 2 compounds are eluted in a reproducible pattern by increasing the organic nature of a buffered mobile phase. Average recoveries of 2,4-dinitro-l-naphthol and 1-naphthol added to samples of Ext. D&C Yellow No. 7 at levels ranging from 0.003 to 0.20% were 103.9 and 94.7%, respectively.

1985 ◽  
Vol 68 (3) ◽  
pp. 471-473
Author(s):  
Robert J Calvey ◽  
Allen L Goldberg

Abstract A sensitive, reproducible method that uses liquid chromatography in the reverse phase mode has been developed for the determination of phthalic acid, resorcinol, and 2-(2',4'-dihydroxybenzoyl)benzoic acid in D&C Yellow No. 7 and D&C Yellow No. 8. The method uses a 10 p, C-8 column, a 1% acetic acid-methanol gradient, and UV absorption detection at 280 nm. Average recoveries of phthalic acid, resorcinol, and 2-(2',4'-dihydroxybenzoyI)benzoic acid were 100, 98, and 1(12%, respectively, from fluorescein standard (certifiable as D&C Yellow No. 7) spiked with each compound at levels ranging from 0.13 to 1.3%.


1985 ◽  
Vol 68 (3) ◽  
pp. 477-479
Author(s):  
Allen L Goldberg

Abstract A sensitive, reproducible method that uses an Extrelut QE column and liquid chromatography (LC) in the reverse phase mode is described forthe determination of 2-(2-quinoIinyl)-l//-indene-l,3-[2JJ]-dione and other organic-soluble matter found in D&C Yellow No. 10. With this method the organic-soluble matter is extracted from D&C Yellow No. 10 on an Extrelut QE column, and the extract is concentrated and analyzed by LC. Recoveries averaged 104% for 2-(2-quinolinyl)-l#- indene-l,3-[2tf]-dione added to purified D&C Yellow No. 10 at levels ranging from 0.50 to 5.96 ppm.


1986 ◽  
Vol 69 (5) ◽  
pp. 915-918
Author(s):  
Edward J Kikta ◽  
◽  
E Bane ◽  
A Burns ◽  
A Christensen ◽  
...  

Abstract A liquid chromatographic (LC) method for the analysis of technical and formulated carbofuran samples was evaluated in a collaborative study. Carbofuran is determined by reverse phase LC, using a water-methanol mobile phase and acetophenone as internal standard, and detected at 280 nm. Twelve samples, 5 formulations and technical matched pairs, were analyzed by 17 collaborating laboratories. Accuracy and variability of results are typical of large LC data sets. The method has been adopted official first action.


1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day

Abstract A residue method is described for determination of the aquatic herbicide fluridone (1-methy1-3-phenyl-5-[3-(trifluoromethyl)phenyl]-4(1H)- pyridinone) and its metabolite (1-methy1-3-(4-hydroxyphenyl)-5-[3- (trifluoromethyl)phenyl]-4(1H)-pyridinone) in fish and crayfish tissues. Both compounds are extracted from tissues with methanol, and the extracts are subjected to acidic hydrolysis to release conjugated forms of fluridone and the metabolite. Sample extracts are purified by liquidliquid partitioning and Florisil Sep-Pak® column chromatography. Both compounds are separated and measured by reverse phase liquid chromatography with UV detection at 313 nm. In the absence of interfering peaks, the method has a detection limit of approximately 0.04 ppm of either compound. Overall, recoveries averaged 96% for fluridone and 78% for the metabolite for all tissue types combined.


1985 ◽  
Vol 68 (4) ◽  
pp. 618-621
Author(s):  
Shih-Ling Yeh-Chen ◽  
Chin-Tan Hsu

Abstract Five methods were investigated for the determination of levulinic acid in soy sauce to determine the addition of protein hydrolysate, mainly acid hydrolysate of defatted soybeans. Best results were obtained by using liquid chromatography (LC) with 0.004M HC104 as the mobile phase and bromcresol purple as a post-column reagent. An innovative LC method with 0.1% H3PO4 as eluant was developed for determination of levulinic acid at 280 nm in soy sauce. This was the most timesaving method.


1989 ◽  
Vol 72 (1) ◽  
pp. 59-59 ◽  
Author(s):  
Delbert D Oehler ◽  
J Allen Miller

Abstract A rapid, sensitive method is described for the determination of ivermectin concentrations in bovine serum. Ivermectin is extracted by passing a sample through a reverse-phase C18 cartridge. A silicapacked cartridge is used to purify the extract further. Ivermectin is quantitated by liquid chromatography with detection at 245 nm. Recoveries were 95 ± 4% for samples fortified with 20 ppb ivermectin. Concentrations as low as 2 ppb can be detected in 5 g samples.


1980 ◽  
Vol 63 (1) ◽  
pp. 91-94 ◽  
Author(s):  
William J Bachman

Abstract Reverse phase high pressure liquid chromatography (HPLC) with ion-pairing is used for the determination of pseudoephedrine hydrochloride in combination with triprolidine hydrochloride or chlorpheniramine maleate in sirups and tablets. Sirups require a preliminary column chromatography cleanup step. Response is linear for pseudoephedrine hydrochloride (range of 0–20 μg), chlorpheniramine maleate (range of 0–1.3 μg), and triprolidine hydrochloride (range of 0–1.0 μg). Recoveries from synthetic formulations were 98.8–101.3% for pseudoephedrine hydrochloride, 100.0–101.2% for chlorpheniramine maleate, and 97.7–99.8% for triprolidine hydrochloride. The coefficient of variation for the method is less than 1%.


1985 ◽  
Vol 68 (4) ◽  
pp. 801-803
Author(s):  
Vinod K Srivastava ◽  
Mohan L Maheshwari

Abstract An isocratic reverse phase liquid chromatographic (LC) system has been developed for qualitative and quantitative assay of morphine, codeine, thebaine, papaverine, and narcotine in gum opium. Five extractions with 2.5% aqueous acetic acid quantitatively extracted the major alkaloids. A mixture of 1% aqueous sodium acetate (pH 6.78), acetonitrile, and 1,4-dioxane (75 + 20 + 5) is used as LC mobile phase | for better resolution of alkaloid peaks, especially those of morphine and codeine. The method is suitable for routine analysis of gum opium I samples.


1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.


1990 ◽  
Vol 73 (3) ◽  
pp. 429-430
Author(s):  
Benny Koppen

Abstract A method Is described for the determination of bromadiolone in rodent bait formulations. Samples are Soxhlet-extracted using methanol as extractant and analyzed by reverse-phase liquid chromatography with UV detection at 280 nm. Chromatography is performed using a ODS-Hypersll (5 fim) column, which enables separation of the 2 diastereolsomers of bromadlolone. The sum of the peak areas of the diastereolsomers Is used for quantitation. The method was tested for precision, linearity, and recovery. Duplicate analyses of 10 formulation samples gave a mean relative standard deviation of 4.1%. Linearity was very good (correlation coefficient 0.9997) In the relevant concentration range. Recovery from spiked samples was 88.9 ±2.3%. The method is applicable to rodent bait formulations with bromadiolone content 0.005% and 0.01%.


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