【求助】求助杀螟硫磷的分析方法

你好！楼主，杀螟硫磷（Sumithion、fenitrothion）的一篇外文检测文献：
Determination of fenitrothion in commercial formulations by square wave voltammetry and UV-Vis spectroscopy
http://www.scielo.br/scielo.php?pid=S0103-50532005000500011&script=sci_arttext&tlng=

以下有一些摘要，如果需要全文，可以去文献求助版求助：
1.Determination of fenitrothion and diazinon in air
Kawata, K | Yasuhara, A
Bulletin of Environmental Contamination and Toxicology. Vol. 52, no. 3, pp. 419-424. 1994

Fenitrothion and diazinon (0,0-diethyl 0-2-isopropyl-6-methyl-pyrimidin-4-yl phosphorothioate) are two pesticides ordinarily used in household, forest and different agricultural pests. Efforts have been made to collect these pesticides in air to determine its atmospheric and environmental effect. Measurement of fenitrothion and diazinon in air by gas chromatography/mass spectrometric utilizing an automated sequential air sampler with activated carbon-fiber filter for collection was presented in this article. In addition, variations of the ground-applied insecticides on lawn was also clarified.

2.Determination of Diazinon and Fenitrothion in Environmental Water and Soil Samples by HPLC
M. E. Snchez; R. Mndez; X. Gmez; J. Martn-Villacorta
Journal of Liquid Chromatography & Related Technologies, Volume 26, Issue 3 March 2003 , pages 483 - 497
Abstract
High performance liquid chromatography (HPLC) methods have been developed for the determination of the organophosphorus pesticides, diazinon, and fenitrothion in environmental water and soil samples; a simple and rapid sample preparation procedure using solid-phase extraction being developed in the case of water samples. In soil samples, the analytical procedure proposed consisted of a 10-min ultrasonic extraction of the target compounds from a 20 g soil sample with 20 mL of acetonitrile and, after centrifugation, the filtering and concentration of the supernatant in an SC110H Speed Vac Plus concentrator to evaporate solvents. The quantification of diazinon and fenitrothion was performed using UV photodiode detection at 245 and 267 nm, respectively. The average recoveries from spiked water and soil samples at various concentration levels exceeded 86% with relative standard deviations of 1.8-5.1%. It was possible to determine concentrations of these pesticides in the range 0.1-2 ng/g in water and soil samples with a good level of reproducibility and accuracy.

3.Determination of dimethoate and fenitrothion in estuarine samples by C-18 solid-phase extraction and high-resolution gas-chromatography with nitrogen-phosphorus detection
V. K. Karamfilovb, a, T. W. Filemanb, K. M. Evansb and R. F. C. Mantoura
Analytica Chimica Acta Volume 335, Issues 1-2, 10 December 1996, Pages 51-61
Abstract
Dimethoate [S-((2-(methylamino)ethyl)-2-oxoethyl)phosphorodithioate] and fenitrothion [O,O-dimethyl O-(4-nitro-m-tolyl)phosphorothioate], both organophosphorus pesticides (OPs), have been successfully enriched on monofunctional C-18 solid-phase extraction (SPE) cartridges and quantified by high-resolution capillary gas-chromatography with nitrogen-phosphorus detection (gc-NPD). The method was optimised for estuarine conditions. The recoveries varied significantly with the pH values of spiked seawater samples in the range pH 6.5–9.0 for both compounds. Salinity did not affect the recoveries of fenitrothion whereas the recoveries of dimethoate increased with salinity. The highest recoveries from water samples spiked at trace concentrations of 100 ng l−1 were 68% and 91% for dimethoate and fenitrothion, respectively, and were achieved at pH 6.5 and a salinity of 36‰. Recoveries from ultrasonically extracted sediments, spiked at 100 ng g−1 dry weight were 91% for dimethoate and 86% for fenitrothion. The detection limits (s/n = 3) for dimethoate and fenitrothion in water and sediment samples were 1 ng l−1 and 2 ng g−1 dry weight, respectively. The reproducibility (RSD) of all determinations was < 10%. Comparison of the gc-EI-MS spectra showed that ions m/z 87,93 and 229 for dimethoate and m/z 109, 260 277 for fenitrothion are suitable for selective ion monitoring. The method was not suitable for extraction and quantification of dimethoxon, an oxygen analogue of dimethoate, as the recoveries were always below 20%. gc column lifetime was significantly improved after calibrations were performed with standard solutions prepared in OP-free extracts of natural samples.

4.Comparison of Soxhlet and Microwave-Assisted Extractions for the Determination of Fenitrothion Residues in Beans
Rokhaya G. Diagne, Gregory D. Foster, and Shahamat U. Khan
J. Agric. Food Chem., 50 (11), 3204 -3207
Abstract:
White and black "niebe" beans [Vigna unguiculata (L.) Walp] from Senegal were treated with fenitrothion (O,O-dimethyl O-4-nitro-m-tolyl phosphorothioate), and the residues were determined by high-performance liquid chromatography (HPLC) and electron capture gas chromatography (EC-gc). Fenitrothion residues from the beans were extracted by Soxhlet extraction (SE) and microwave-assisted extraction (MAE). A column cleanup procedure was used to remove the coextractives in the extract before HPLC and EC-gc analyses. The overall mean recoveries of fenitrothion residues in the 0.19-1.90 g/kg fortification range determined from extracts obtained by SE and MAE were 88.4 and 89.8%, respectively, with respective relative standard deviations of <4%. The results show that MAE is a viable alternative to the commonly used SE for the determination of fenitrothion residues in beans.

5.Identification and Determination of Fenitrothion Photolysis Products in Water-Methanol by Gas Chromatography-Mass Spectrometry
Durand, G | Mansour, M | Barcelo, D
Analytica Chimica Acta ACACAM, Vol. 262, No. 1, p 167-178, June 1992. 3 fig, 2 tab.

The photodegradation of fenitrothion was examined in distilled water containing methanol. After 7 hr of UV irradiation with a high-pressure mercury lamp, a fractionation step was carried out on a semi-preparative silica gel column. Eighty-eight fractions were collected by increasing the polarity of an eluent mixture of n-hexane-ethyl acetate (95+5) up to 100% ethyl acetate. Three more polar fractions in eluent mixtures of n-hexane-acetone (50+50), pure acetone and acetone-methanol (25+75) were obtained. The breakdown products formed were identified by gas chromatography-mass spectrometry with electron impact (EI) ionization. An estimate of the amount of fenitrothion degraded indicated that after 7 hr of irradiation, 10% of the parent compound still remained and different oxidation, isomerization and solvolysis products were produced. The P=S group was oxidized to give fenitrooxon and trimethyl phosphate in amounts of 0.1% and 3%, respectively. Carbomethyoxyfenitrothion, due to oxidation followed by solvolysis, and the isomerization products O,O,S-trimethyl phosphorothioate and the S-methyl isomer of fenitrothion were obtained as photoalteration products at 10%, 10% and 3%, respectively. Other compounds corresponded to denitrofenitrothion, carbomethoxydenitrofenitrothion, parathion-methyl and 4-nitro-m-cresol at 0.2%, 0.4% and 0.4%, respectively. The EI mass spectra and the structures of the ions of the different fenitrothion photolysis products are given.

6. Selective Extraction and Determination of Multiclass Pesticide Residues in Post-Harvest French Beans by Low-Pressure Gas Chromatography/Tandem Mass Spectrometry
附件

你好！以上这些主要还是残留检测方面的，有效成分分析文献有中文的：
20%杀螟硫磷水乳剂的高效液相色谱分析研究；
甲萘威·杀螟硫磷复配制剂的气相色谱同柱检测
杀螟硫磷的高效液相色谱分析方法

谢谢版主的帮忙，残留的分析： 要知道分析的方法， 仪器，试剂，分析的操作过程，计算公式。。

有效成分的分析：杀螟硫磷的高效液相色谱分析方法 这篇文章希望版主帮忙。。。