Liquid Chromatographic Determination of Bromadiolone in Rodent Baits

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%.

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.


1987 ◽  
Vol 70 (6) ◽  
pp. 1058-1059
Author(s):  
Connie C Gehrig ◽  
Rodger W Stringham

Abstract Cholecalciferol (vitamin D3) is extracted In acetonitrile on a Goldfisch apparatus, diluted to volume, and determined by reverse phase liquid chromatography (LC). The sum of the peak heights of pre-vitamin D3, and cfr-vitamin D3, is used for quantitation. The method was tested for precision, linearity, and recovery. Quadruplicate analyses of 5 formulation samples gave relative standard deviations of 1.56- 2.65%. Linearity was excellent with regression and correlation coefficients of 0.9997 and 0.9998, respectively. Recovery was 98.0 ± 2.7%. The method is applicable to 0.075% cholecalciferol rodent baits.


1985 ◽  
Vol 68 (5) ◽  
pp. 950-951 ◽  
Author(s):  
Pedro Rafael Forbito ◽  
Norma Elena Babsky

Abstract A rapid method is described for the quantitative determination of patulin in apple juice. The mycotoxin is extracted from the sample with ethyl acetate and the extract is cleaned up by extraction with a sodium carbonate solution. Patulin is determined by reverse phase liquid chromatography using a μ.Bondapak C18covery is >75%.


1986 ◽  
Vol 69 (3) ◽  
pp. 478-482
Author(s):  
Alan L Scher ◽  
H Dean Murray

Abstract Methods are described for the determination of leuco base in FD&C Blue No. 1 by reverse phase liquid chromatography and for the preparation and standardization of leuco base stock solution. The stock solution is prepared by reductive titration of the color with TiCl3. Solutions of the color and of leuco base are chromatographed by isocratic elution, which is followed by a wash and equilibration that can be omitted for screening. Peak area and height calibrations were linear. At the specification level, the 99% prediction limits were 5.00 ± 0.14% (area) and 5.00 ± 0.37% (height). Limits of determination were 0.29% (area) and 0.73% (height) at the 99.5% confidence level. Recoveries were 97-101% for leuco base added to FD&C Blue No. 1 at levels of 1-6%.


1989 ◽  
Vol 72 (2) ◽  
pp. 231-234 ◽  
Author(s):  
Mercedes Jalón ◽  
Majesús Peńa ◽  
Julián C Rivas

Abstract A reverse-phase liquid chromatographic method is described for the determination of carminic acid in yogurt. A C18 column is used with acetonitrile-1.19M formic acid (19 + 81) as mobile phase and diode array detection. Sample preparation includes deproteinization with papain and purification in a polyamide column. The relative standard deviation for repeated determinations of carminic acid in a commercial strawberry-flavored yogurt was 3.0%. Recoveries of carminic acid added to a natural-flavored yogurt ranged from 87.2 to 95.3% with a mean of 90.2%. The method permits measurement of amounts as low as 0.10 mg/kg.


1989 ◽  
Vol 72 (6) ◽  
pp. 1007-1009
Author(s):  
Vipin K AGARWAL

Abstract A method is described for the determination of vitamins D2 + D3 in milk- and soy-based infant formula. Vitamins D2 and D3 are extracted from the saponified sample and converted to isotachysterols with acidified butanol. Reverse-phase liquid chromatography (LC) is used to remove interferences, and total vitamin D is quantitated using normal-phase LC. Recoveries of spiked samples averaged 97.6% for milk-based infant formula, and 98.8% for soy-based infant formula. This method quantitates vitamin D2 + D3 in infant formulas containing as low as 40 IU/qt when prepared according to label direction


1990 ◽  
Vol 73 (5) ◽  
pp. 753-761 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters

Abstract A method Is described for determining residues in foods of thiabendazole, thlophanate methyl, the dl-oxygen analogue metabolite [dimethyl 4,4'-0-phenylene bis (allophanate)] that Is the metabolite name of the latter, and methyl-2- benzlmldazole carbamate, which Is the major metabolite and fungltoxlc principle common to both thlophanate methyl and benomyl. The residues are extracted from the product using methanol and are partitioned Into dlchloromethane after initial acidification and again after subsequent alkalinization of the extract. Residues are separated and quantified by reverse- phase liquid chromatography using an ion-pairing mobile phase with UV and fluorescence detectors In tandem. Recoveries from 7 different food crops fortified at 0.2-35 ppm levels ranged from 64 to 105%.


1984 ◽  
Vol 67 (5) ◽  
pp. 861-862 ◽  
Author(s):  
John Morawski ◽  
Glenn Kyle

Abstract A rapid, reliable separation and quantitation of zoalene (3,5-dinitroo-toluamide) from feeds is accomplished by using reverse phase liquid chromatography (LC) and ultraviolet detection. An extraction technique which is similar to the present AOAC official colorimetric method is used before chromatographic analysis. This extraction is followed by an activated alumina cleanup and LC to separate zoalene from feed matrix. The methodology was applied to a variety of spiked feed matrices, and yielded good recoveries. Liquid chromatographic results were shown to correlate with colorimetric determinations.


1988 ◽  
Vol 71 (3) ◽  
pp. 462-465
Author(s):  
Pietro Damiani ◽  
Giovanni Burini

Abstract Two procedures, one fluorometric and the other reverse phase liquid chromatographic, for determination of a derivative of diacetyl are described. Exploratory work on diacetyl standard solutions to establish the best conditions for the derivatization with 2,3-diaminonaphthalene (DAN) to yield 2,3-dimethylbenzo[g]-quinoxaline (DMBQ) is discussed, as well as the fluorescence characteristics of the DMBQ derivative. Diacetyl was determined in 10 commercial butter samples by the proposed procedures and by other known methods (determination of o-phenylenediamine and 3,3-diaminobenzidinederivatives). Recoveries from butter samples spiked with known amounts of diacetyl ranged from 96.9 to 101.8% (with CVs ranging from 0.3 to 2.1%) for the fluorometric procedure and from 96.9 to 102.7% (with CVs ranging from 0.5 to 2.4%) for the chromatographic procedure. These results agree well with those obtained with o-phenylenediamine and 3,3-diaminobenzidine methods on the same butter samples. The proposed methods have the advantages of improved detectability and specificity.


1982 ◽  
Vol 65 (4) ◽  
pp. 927-929
Author(s):  
Brian R Bennett ◽  
Gregory S Grimes

Abstract Chlorophacinone and diphacinone are extracted at the 0.005% level from grain or paraffinized baits with glacial acetic acid. The target concentration is 0.01 mg/mL. The filtered supernate is chromatographed on a Partisil PXS ODS10/25 liquid chromatography column with premixed and degassed glacial acetic acid-tetrahydrofuran-water (14 + 2 + 9) and detected at 288 nm. The concentration is calculated by using an external standard. The recovery from spiked samples averaged 96.6% for both analytes. The response is linear from 0.001 to 0.040 mg/mL. The coefficient of variation of within-day replicates ranged from 1.1 to 2.5%.


Sign in / Sign up

Export Citation Format

Share Document