Gas chromatographic and high performance liquid chromatographic determination of d-phenothrin (Sumithrin) in formulations.

Sakaue, Shigeyuki; Kitajima, Megumi; Horiba, Masao; Yamamoto, Seiya

doi:10.1271/bbb1961.45.1135

Cited by 7 publications

(3 citation statements)

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“…The Ministry of Health and Welfare investigated the amounts of phenothrin residues in food imports after the sprayings in order to insure safety. There are a few reports (6) on analysis of phenothrin in foods, but adequate detection sensitivity has not been obtained owing to the mechanical limitations of gas chromatography (GC) with flame ionization detection (FID) or high pressure liquid chromatography (HPLC) with uv detection or GC with a packed column. Therefore, the authors sought to develop a more sensitive method for analyzing phenothrin using gas chromatography with electron capture detection (ECD-GC) and ion-trap GC with mass spectrometry (ion-trap GC/MS), and to apply the method to imported samples sprayed with phenothrin.…”

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Analysis of Phenothrin and Its Metabolite 3-Phenoxybenzoic Acid (PBA) in Agricultural Products by GC and Ion-Trap GC/MS

Hirahara¹,

Tsumura

Nakamura

et al. 1997

Journal of Food Protection

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A sensitive method for analysis of phenothrin and its metabolite 3-phenoxybenzoic acid (PBA) in agricultural products by gas chromatography with electron capture detection (ECD-GC) and ion-trap gas chromatography/mass spectrometry (GC/MS) with chemical ionization (Cl) was investigated. After phenothrin in vegetables, fruits, potatoes, starches, and tea had been extracted with acetone, or in cereals and beans had been extracted with acetonitrile followed by Florisi! column chromatography, it was reextracted into n-hexane. PBA was determined by ECD-GC after esterification with hexafluoroisopropyl alcohol (HFIP) and diisopropylcarbodiimide (DIC). Phenothrin was determined by monitoring its molecular ion peak using ion-trap GC/MS and was confirmed by observing its spectral pattern. The detection limit for phenothrin by ECD-GC and ion-trap GC/MS by this method was 0.01 ppm. The detection limit for PBA by ECD-GC was 0.001 ppm. When phenothrin and PBA were added to samples at 0.2 and 1.0 ppm, the recoveries of phenothrin in each agricultural product ranged between 60.2 and 88.5% and those of PBA ranged between 37.8 and 89.5%. An actual-conditions surveillance analysis of six agricultural products imported from October to December 1994 indicated no phenothrin, but PBA was detected in all products.

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Analysis of Phenothrin and Its Metabolite 3-Phenoxybenzoic Acid (PBA) in Agricultural Products by GC and Ion-Trap GC/MS

Hirahara¹,

Tsumura

Nakamura

et al. 1997

Journal of Food Protection

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“…Previous literature studies have been directed toward the determination of piperonyl butoxide in the presence of pyrethroid and other insecticides. For example, direct derivative UV , and fluorescence spectrophotometry, gas chromatography with flame ionization detection, and liquid chromatography with UV 2,16 or fluorescence detection methods have been successfully developed. Haddad et al have calculated a detection limit of 3.0 × 10 -6 M for piperonyl butoxide on rice using HPLC with UV detection.…”

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confidence: 99%

Electrochemical Behavior and Determination of the Insecticide Synergist Piperonyl Butoxide

1997

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Piperonyl butoxide may be reversibly oxidized in acetonitrile at a glassy carbon electrode to a cation radical under short time scale voltammetric conditions, e.g., cyclic voltammetry when the potential scan rate is above 500 mV s(-)(1). During longer time domain experiments, the cation radical decays in a rate-limiting heterolytic bond cleavage step and subsequent transfer of a second electron at the potential of the first process. Additionally, a second oxidation process develops at more positive potentials. One product isolated from the initial oxidation process in an almost quantitative yield, under controlled potential electrolysis conditions, is 6-n-propyl-1,3-benzodioxole-5-carboxaldehyde. This carboxaldehyde is oxidized at the same positive applied potential as the second oxidation process observed in long time domain voltammetric experiments with piperonyl butoxide. The limit of detection for piperonyl butoxide in acetonitrile, using differential pulse voltammetry at a glassy carbon electrode, is 1.6 × 10(-)(6) M (3σ), with a limit of determination of 4.1 × 10(-)(6) M (10σ). Piperonyl butoxide was selectively determined using differential pulse voltammetry with a concentration of 5.11 ± 0.02 g L(-)(1) in a commercial insecticide formulation containing pyrethrins. This result is in good agreement with the manufacturer's stated concentration of 5.07 g L(-)(1). The sample preparation requires only simple dilution of the formulation in an acetonitrile/dichloromethane (95:5) solvent mixture.

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“…A broad linear range for the analysis was required because the dissipation rate of the d-phenothrin formulation from the bath solutions was to be monitored so that an effective deposition of active ingredient could be made. A method for gas chromatographic and high-performance liquid chromatographic determination of d-phenothrin in formulations by Sakaue et al (1981) was not satisfactory because they assayed formulations only at the 1 mg/mL concentration level and did not use any cleanup procedures to remove interferences at the low concentration ranges we needed to measure. Desmarchelier (1980) used a colorimetric procedure to determine residues.…”

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Rapid extraction and gas-liquid chromatographic determination of d-phenothrin in aqueous formulations

Simonaitis¹,

Cail²

1988

J. Agric. Food Chem.

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Gas chromatographic and high performance liquid chromatographic determination of d-phenothrin (Sumithrin) in formulations.

Cited by 7 publications

References 0 publications

Analysis of Phenothrin and Its Metabolite 3-Phenoxybenzoic Acid (PBA) in Agricultural Products by GC and Ion-Trap GC/MS

Analysis of Phenothrin and Its Metabolite 3-Phenoxybenzoic Acid (PBA) in Agricultural Products by GC and Ion-Trap GC/MS

Electrochemical Behavior and Determination of the Insecticide Synergist Piperonyl Butoxide

Rapid extraction and gas-liquid chromatographic determination of d-phenothrin in aqueous formulations

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