Liquid Chromatographic Determination of Pyrethroids as Active Ingredients in Pesticide Formulations

1994 ◽  
Vol 77 (4) ◽  
pp. 810-814 ◽  
Author(s):  
Benny Koppen

Abstract A normal-phase liquid chromatographic method for determining pyrethroids as active ingredients in pesticide formulations was developed. The method uses isooctane–ethyl acetate as mobile phase and UV detection at 275 nm. The method was evaluated for the following 7 pyrethroid active ingredients: α-cypermethrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, and permethrin. Evaluation covered 3 formulation types (emulsifiable concentrate, suspension concentrate, and water-dispersible granule) containing a single pyrethroid active ingredient. The method separates diastereomers of cypermethrin, fenvalerate, and permethrin and can be used to determine total content as well as relative distribution of diastereomers.

1985 ◽  
Vol 68 (6) ◽  
pp. 1134-1136 ◽  
Author(s):  
Rodney J Bushway

Abstract A liquid chromatographic method has been developed to quantitate pyrethrins in pesticide formulations. Samples were dissolved in tetrahydrofuran (THF) and injected onto an amino column with a solvent system of hexane-nonstabilized THF (90 + 10) at a flow rate of 1.5 mL/min. Detection was monitored at 240 nm and 0.4 AUFS. Total elution time was 7 min. Twelve products varying in concentration from 0.05 to 3.75% and formulated with numerous other ingredients were analyzed. Percent coefficients of variation ranged from 1.39 to 9.68 with the majority less than 5.00. Although piperonyl butoxide and Noctyl bicycloheptene dicarboximide (MGK 264) were not quantitated, neither interfered with the pyrethrin analysis


1985 ◽  
Vol 68 (3) ◽  
pp. 580-582
Author(s):  
Rodney J Bushway ◽  
Harold Johnson ◽  
Donald W Scott

Abstract This paper describes a reverse phase liquid chromatographic (LC) method to simultaneously determine rotenone and pyrethrins in pesticide formulations. The mixed standards along with the formulations were accurately weighed to contain approximately 200 (μg rotenone and 150 (μg pyrethrins/mL. Stabilized tetrahydrofuran was used to dissolve all substances. An aliquot was injected into the LC system equipped with a Zorbax ODS column, and chromatographed with a mobile phase of acetonitrile-water (70 + 30). Rotenone and the pyrethrins were monitored at 240 nm and 0.4 AUFS. Retention times for rotenone, pyrethrin II, and pyrethrin I were approximately 7, 11.5, and 25.5 min, respectively. For 3 different formulations analyzed 6 times each, the percent coefficients of variation were all < 3. This method is also applicable to products containing either rotenone or pyrethrins. No significant interferences were observed from the inactive ingredients of the formulations at the concentrations added.


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.


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%.


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.


1983 ◽  
Vol 66 (3) ◽  
pp. 663-666
Author(s):  
Ijaz Ahmad

Abstract A simple and fast analytical method is described for the quantitative determination of low levels of paraquat residues in water. The method involves extraction and concentration of paraquat in water by using a C18 Sep-Pak cartridge followed by reverse phase high performance liquid chromatographic determination with ultraviolet detection at 257 nm. Recoveries of paraquat from spiked samples were above 93% with a coefficient of variation of 6.1%. The method can be used for water samples with paraquat concentrations as low as 0.05 ppm.


1995 ◽  
Vol 78 (2) ◽  
pp. 307-309 ◽  
Author(s):  
Theresa A Gehring ◽  
Willie M Cooper ◽  
Claude L Holder ◽  
Harold C Thompson

Abstract A liquid chromatographic method was developed for determination of the essential nutrient thiamine (vitamin Bi) in rodent feed. Thiamine was extracted with hydrochloric acid, separated by reversed-phase liquid chromatography, derivatized postcolumn to thiochrome with potassium hydroxide and potassium ferricyanide, and detected by fluorescence. Excitation and emission wavelengths were 370 and 430 nm, respectively. Detector response was linear in the range of 2.58 to 15.5 ng of thiamine injected. Instrument detection limit was 5 pg of thiamine injected.


1994 ◽  
Vol 77 (5) ◽  
pp. 1175-1179 ◽  
Author(s):  
Ghulam Sarwar ◽  
Herbert G Botting

Abstract A reversed-phase liquid chromatographic (LC) method involving precolumn derivatization with phenylisothiocyanate (PITC) was developed for determining levels of hypoglycin A (HG-A) in canned ackee fruit samples. HG-A was extracted by homogenizing the drained fruit in 80% ethanol. By using a Waters Pico-Tag amino acid analysis 15-cm-long column (which is also used for analyzing protein hydrolysates and biological samples) and an LC system, the baseline separation of HG-A from other amino acids was completed in about 6 min. The total time for analysis and equilibration was 16 min. HG-A levels in the edible portion of fruit in 18 cans varied from 18.27 to 87.50 mg HG-A/can. Recoveries of added standard HG-A averaged 101%. To our knowledge, this is the first report of the use of this method to determine HG-A in ackee fruit.


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.


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