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1.
A wide range of crops including top fruit, cereals, brassicas, root vegetables and cotton from field trials in several countries in 1965, 1966, 1967 and 1968 have been analysed for residues of tetrachlorvinphos (Gardona, trans-homer of dimethyl 1-(2′,4′,5′-trichlorophenyl)-2-chlorovinyl phosphate) foliar insecticide, its isomer and its potential breakdown products. The residues under field conditions were mainly of tetrachlorvinphos, its isomer and 1-(2′,4′,5′-trichlorophenyl)ethan-1-ol in free and sugar-conjugated forms. Tetrachlorvinphos was not unduly persistent on the crops and its initial half-life varied from 2 days on cabbage, to 7 days on potato foliage and to 12 days on pears (after the last of five applications). From one week after the final application onwards the highest residues of tetrachlorvinphos observed were on olives (1 ppm after 18 days after a single application of 0·1 % active material), maize leaf (2·8 ppm at 9·5 weeks after the last of two applications at 3 kg/ha), and cabbage (1·9 ppm at 12 days after the last of three applications at 0·5 kg/ha). The maximum residues of the alcohol in the free form were 3·2 ppm on maize leaf at 8 weeks from the second application at 1·5 kg/ha and in the conjugated form were 1·0 ppm on cauliflowers at 6 days after the last of four applications at 0·5 kg/ha. 相似文献
2.
Methods are described for the analysis of residues of the herbicide benzoylpropethyl, ethyl (±)-2-[ N-(3,4-dichlorophenyl)benzamido]propionate, and its breakdown product, (±)-2-[ N-(3,4-dichlorophenyl)benzamido]propionic acid, in wheat and soil. In wheat the acid degradation product conjugates with plant sugars and the present paper includes methods for determination of these residues either separately or as a combined residue with unconjugated acid. Efficient extraction procedures have been developed together with partition and column chromatographic techniques for purification of extracts. The full analytical procedures are described and the final determinations are by g.1.c. with electron capture detection with blank values for field samples in the range 0.01–0.05 mg/kg. Good recoveries were obtained. Radiochemical techniques have been used to verify the extraction and subsequent procedures in the methods. 相似文献
3.
Apples treated with tetrachlorvinphos (Gardona, trans-isomer of dimethyl 1-(2′,4′,5′-trichloropheny1)-2-chlorovinyl phosphate) insecticide under field conditions in several countries in 1965, 1966 and 1967 have been analysed at intervals after treatment for residues of tetrachlorvinphos itself, its cis-isomer and seven potential breakdown products. Residues of up to 10 ppm of tetrachlorvinphos were detected immediately after the last of three applications of tetrachlorvinphos (diluted to 0.16% active material). The initial half-life of the tetrachlorvinphos was on average about 0.5 weeks under U.K. conditions and only 10% of the tetrachlorvinphos remained unchanged at 2 weeks after application. The overall chemical persistence of the wettable powder formulation was not significantly different from that of the emulsifiable concentrate formulation. Within 8 weeks of the application the residues were mainly of tetrachlorvinphos itself, its cis-isomer and the alcohol 1-(2′,4′-5′-trichlorophenyl)ethan-l-ol, in free and sugar-conjugated forms. The residues of the conjugates of this alcohol (up to 0.92 ppm) were generally present in higher concentration at 6-8 weeks after the application than were the residues of the other components. Whilst residues of other breakdown products were detected on the apples their individual residues were below 0.05 ppm and generally below 0.01 ppm at 6 weeks or more after the last of several applications of tetrachlorvinphos. 相似文献
4.
K. I. Beynon 《Pest management science》1972,3(4):389-400
Radiochemical techniques have been used to develop efficient procedures for the extraction of residues of cyanazine herbicide [‘BLADEX’, 1 BLADEX and FORTROL are Shell registered Trade Marks. a ‘FORTROL’,a 2-chloro-4-(1-cyano-1-methylethylamino)-6-ethylamino-1,3,5-triazine] and its metabolites 2-chloro-4-(1-carbamoyl-1-methylethylamino)-6-ethylamino-1,3,5-triazine ( II ), 2-chloro-4-(1-cyano-1-methylethylamino)-6-amino-1,3,5-triazine ( V ) and 2-chloro-4-(1-carbamoyl-1-methylethylamino)-6-amino-1,3,5-triazine ( VI ) from crops and soils. Partition and column chromatographic techniques have been established for the purification of the extracts. The full analytical procedure is described and the final determination of all four compounds is by g.l.c. with electron capture detection with blank values for field samples generally 0.02 part/million and with good recoveries. 相似文献
5.
Patricia K. Johnstone Ian R. Minchinton Roger J. W. Truscott 《Pest management science》1985,16(2):159-162
A method is described for the analysis of soils for residues of the herbicide diclofop-methyl, methyl (RS)-2-[4-(2,4-dichlorophenoxy)phenoxy]propionate, and its breakdown product diclofop, (RS)-2-[4-(2,4-dichlorophenoxy)phenoxy]propionic acid. Diclofop-methyl undergoes hydrolysis in the soil to diclofop, which also has herbicidal activity. A procedure, using a 1% phosphoric acid solution for extraction purposes, has been developed and gives good recoveries of both diclofop-methyl and diclofop at the 0.5 and 0.05 mg kg?1 levels. After methylation, gas-liquid chromatography with electron-capture detection is used to determine total residue concentrations. 相似文献
6.
Extractable residues of endosulfan stereoisomers and its toxic metabolite, endosulfan sulfate, on a vegetable, an oilseed and a pulse crop were determined by gas-liquid chromatography. The study revealed that the alpha isomer degraded faster than the beta isomer. Beta-endosulfan accumulated during the first three days following the treatment. Endosulfan sulfate residues appeared a few days after application and decreased with time. The total endosulfan residues in the seeds from treated mustard ranged from 0.08 to 0.12 mg kg?1 and were at or below the limit of determination (0.02 mg kg?1) in chickpea seeds following harvest. 相似文献
7.
A procedure has been developed for the analysis of crops and soils for residues of trifenmorph (N-trityl-morpholine) molluscicide and its breakdown product triphenylcarbinol (TPC). Samples were extracted with 20% by vol. acetone in petroleum ether and the efficiency of the extraction was established using radiochemical techniques. The extracts were subjected to column chromatography on basic alumina columns to separate trifenmorph from the TPC. The residues were converted to trichloroethyl ether derivatives followed by clean-up by column chromatography on silica gel and analysis of down to 0·02 ng by gas-liquid chromatography. Blank values were generally 0·01–0·02 ppm, recoveries were on average about 80% and were limited to this value by the yield of the etherification reaction. The storage stability of the residues at —10°c was satisfactory. 相似文献
8.
W. J. Allender 《Pest management science》1990,29(2):183-186
A method is described for the measurement of simazine [2-chloro-4,6-bis(ethylamino)-1,3,5-triazine] residues in chickpeas (Cicer arietinum). Ground chickpea samples were extracted with dichloromethane, followed by clean-up on alumina. Gas-liquid chromatography using metribuzin [4-amino- 6-tert-butyl-4,5-dihydro-3-methylthio-1,2,4-triazin-5-one] as internal standard with thermionic detection was used to quantify simazine residues. The limit of detection was 0.02 mg kg?1 and the recoveries of simazine from chickpea samples (0.1–4 mg kg-1) averaged 92%. 相似文献
9.
Thin-layer and gas-liquid chromatography, ultraviolet analysis and bioassay with Chlorella spp. have been used to investigate the pathway of degradation of diuron to phytotoxic derivatives when diuron was used as a soil-residual herbicide in irrigation canals. Observations suggest that 1-(3,4-dichlorophenyl)-3-methylurea and 1-(3,4-dichlorophenyl)urea make a contribution to total residues equivalent to a maximum of about 40 and 55%, respectively, of diuron concentrations. Application of a phyto-toxicity rating suggests that in this environment, measurement of diuron specifically would underestimate the total phytotoxicity of residues by a maximum of about 7%. 相似文献
10.
An improved method for the analysis of carbofuran residues and its metabolites in plant material has been developed. Critical evaluation of previously published methods has enabled the elimination of unnecessary procedures, and practical difficulties have been overcome or minimised without loss of sensitivity. Separate extraction of bound and non-bound residues is followed by clean-up by coagulation, preparation of a derivative with 1-fluoro-2,4-dinitrobenzene, and gas-liquid chromatography using a thermionic nitrogen-selective detector system. The method can be used in general screening for carbamates as well as analysis for specific carbamate pesticide residues. 相似文献
11.
Crops and soils from field trials in 1967–1970 in several countries have been analysed for residues of the triazine herbicide cyanazine (‘BLADEX’ 1 Shell Registered Trade Mark. a or ‘FORTROL’a' 2-chloro-4-(1-cyano-1-methylethylamino)-6-ethylamino-1,3,5-triazine) and for its degradation products 2-chloro-4-(1-carbarmoyl-1-methylethylamino)-6-ethylamino-1,3,5-triazine ( II ), 2-chloro-4-(1-cyano-1-methylethylamino)-6-amino-1,3,5-triazine ( V ) and 2-chloro-4-(1-carbonyl-1-methylethylamino)-6-amino-1,3,5-triazine ( VI ). The time for the concentration of cyanazine in soils to fall to half the initial value was in the range 1.3 to 5 weeks with a mean value of 2.4 weeks. The rate of loss was not affected by sparse crop cover and there was some indication that the rate was greater under moist soil conditions. Residues of up to 0.5 part/million of ( II ) and up to 0.08 part/million of ( VI ) were detected in soils at 4 weeks from cyanazine application at 2 kg/ha. The residues of cyanazine and the degradation products declined rapidly and were 0.07 part/million or less at 16 weeks from treatment. Repeated annual applications did not lead to a detectable build up of residues in soil. Neither residues of cyanazine nor those of ( II ), ( V ) or ( VI ) could be detected in a wide range of crops harvested from soil treated in accordance with the likely recommendations and the limits of detectability were 0.01 to 0.04 part/million. 相似文献
12.
The non-extractable residues of the fungicide cyprodinil formed in heterotrophic cell suspension cultures of wheat were studied by application of [2-pyrimidyl-14C] or [2-pyrimidyl-13C]cyprodinil. The main objective was to examine whether solid-state and liquid 13C NMR spectroscopy can be used to examine plant bound residues of pesticides. For 14C experiments, wheat suspensions grown on glucose as carbon source were treated with 10 mg litre(-1) of 14C-cyprodinil. After incubation for 12 days, 20% of applied 14C was detected as non-extractable residues. The cell debris were treated with 0.1 M HCl (reflux), 1.0 M HCl (reflux), buffer, or 2 M NaOH (50 degrees C); Bj?rkman lignin and acidolysis lignin fractions were also prepared from the debris. Radioactivity liberated and solubilized by these procedures was examined by thin-layer chromatography and high-performance liquid chromatography. The results showed that cyprodinil and primary metabolites contributed to the fungicide's bound residues. Most of the residues (12% of applied 14C) remained associated with polar or polymeric/oligomeric endogenous cell materials in a stable manner. For the study with 13C-cyprodinil, wheat suspensions were cultivated on 13C-depleted glucose for four growth cycles, resulting in maximum 13C depletion of the natural cell components to about 0.10%. During the fourth cycle, 13C-labelled cyprodinil was applied, and cells were incubated (12 days). Cell debris was prepared and examined by solid-state 13C NMR spectroscopy. Debris was then treated as described above in the 14C experiment. Solubilized fractions were analyzed by liquid 13C NMR spectroscopy. However, none of the 13C NMR spectra recorded gave utilizable or unambiguous results, and all exhibited large inconsistencies, especially concerning the data from the conventional 14C experiment. 相似文献
13.
氯溴异氰尿酸在烟叶及其土壤中的残留分析及消解动态 总被引：1，自引：1，他引：0
建立了烟叶及其土壤中氯溴异氰尿酸残留的检测方法,并测定了氯溴异氰尿酸在烟叶及其土壤中的消解动态和最终残留。样品经乙腈提取,三氯甲烷、石油醚萃取后,采用高效液相色谱(HPLC-UV)检测。结果表明:在0.01~0.5 mg/kg添加水平下,氯溴异氰尿酸在鲜烟叶、干烟叶和土壤中的平均回收率分别为82.7% ~91.6%、89.2% ~91.8%和89.2% ~94.4%,相对标准偏差(RSD)分别为1.1% ~3.9%、2.6% ~5.5%和1.5% ~4.6%,方法的检出限(LOD)均为0.003 mg/kg, 定量限(LOQ)均为0.01 mg/kg。田间消解动态结果表明,氯溴异氰尿酸在烟叶及其土壤中消解较快,半衰期分别为3.94~4.25 d和2.83~3.41d,施药后14d,其在烟叶和土壤中的消解率均达90%以上。氯溴异氰尿酸可湿性粉剂按有效成分600 g/hm2(推荐高剂量)和900 g/hm2(1.5倍推荐高剂量)于烟草现蕾期对水喷雾施药3~4次,距末次施药后间隔21d采样,烟叶中氯溴异氰尿酸的残留量为1.47~3.52 mg/kg,土壤中的残留量为未检出~0.43 mg/kg。 相似文献
14.
Baldwyn Torto Yousif O
H Assad Peter G
N Njagi Ahmed Hassanali 《Pest management science》1999,55(5):570-571
Bioassays have shown that sand freshly contaminated by ovipositing females of the gregarious desert locust Schistocerca gregaria (Forskal) is more effective in inducing further oviposition from conspecifics than contaminated sand stored for three or six months, which contrasts with results obtained previously with Locusta migratoria (Reiche & Farmaire). The activity of contaminated sand correlated with the levels of three unsaturated aliphatic ketones, (Z)-6-octen-2-one, (E,E)-3,5-octadien-2-one and its geometric isomer (E,Z)-3,5-octadien-2-one present in the volatile emissions from the sand. 相似文献
15.
Five agricultural crops were treated with OO-diethyl O-(3,5,6-trichloro-2-pyridyl) phosphorothioate (chlorpyrifos) granular or emulsifiable concentrate formulations at dosages from 0.5 to 6.0 kg (a.i.)/ha and at different periods before harvest. Chlorpyrifos residues were determined by gas chromatography after extraction and sweep co-distillation clean-up. Low residue levels were found. The average values in lettuce were 0.046 and 0.070 part/million, in sugar beet leaves 0.037 to 0.128 part/million and roots <0.005 to 0.038 part/million; no chlorpyrifos was detected in carrots, potatoes and cured tobacco leaves at the limit of the method (0.005 part/million). 相似文献
16.
Two procedures are described for the determination of residues of triadimenol and compared on cereal material. After extraction, purification is carried out by Florisil column chromatography in method I and by semi-preparative High-Performance Liquid Chromatography in method II. Triadimenol residues are quantified by gas chromatography with a thermoionic detector. With method I, interference was observed but not with method II. This specific procedure has been tested on other plant materials. Recoveries in the range of 90–98% indicate that this procedure is suitable for residue analysis of this fungicide with detection limits of 0·008 mg kg?1 in wheat grains, 0·03 mg kg?1 in wheat straw and 0·004–0·008 mg kg?1 in other plants. Maximum residue limits in France are: 0·1 mg kg?1 in grain, 2·0 mg kg?1 in straw and 1·0 mg kg?1 in other vegetables and fruit. 相似文献
17.
Stephen T. Hadfield Jill K. Sadler Elek Bolygo Ian R. Hill 《Pest management science》1992,34(3):207-213
This paper describes the development of methods suitable for the sampling and analysis of the pyrethroid insecticides lambda-cyhalothrin and cypermethrin in natural waters. A solid-phase water-sampling method which avoids the requirement for transport and storage of large volumes of water is described. This method is shown to be capable of extracting trace levels (ng litre?-1) of the title compounds from natural waters with efficiencies of at least 80%. Chromatographic analysis of processed samples by gas chromatography–electron capture detection enables determination of residues at levels of 1–2 ng litre?-1 in water. 相似文献
18.
Michel Couderchet Pierre F. Bocion Reynold Chollet Karl Seckinger Peter Bger 《Pest management science》1997,50(3):221-227
Due to the presence of an asymmetrically substituted C atom, dimethenamid [2-chloro-N-(2,4-dimethyl-3-thienyl)-N-(2-methoxy-1-methylethyl)acetamide], a recently introduced N-thienyl chloroacetamide herbicide, exists as two stereoisomers (S and R) having differing herbicidal activities as demonstrated with a selection of weeds and Lemna minor. The activity of the two isomers was investigated in greater detail with the green alga Scenedesmus acutus and compared to that of alachlor [2-chloro-N-(2,6-diethylphenyl)-N-(methoxymethyl)acetamide]. As with alachlor, the S isomer (5 μM ) strongly inhibited algal growth and fatty acid desaturation while the R isomer had no effect. In short-term experiments (up to 5·5 h), the S isomer and alachlor (100 μM ) inhibited [14C]acetate uptake and its incorporation into fatty acids in the same manner, while the R isomer did not. Incorporation of [14C]acetate into a non-lipid fraction of the algae was strongly inhibited by alachlor and the S isomer (100 μM ) and only slightly by the R isomer. A 50% inhibition of incorporation of [14C]oleic acid into the same non-lipid fraction was attained with less than 10-7 M of the S isomer while 10-5 M of the R form of dimethenamid achieved only a 40% inhibition. The same stereospecificity of the compound on growth, fatty acid desaturation, acetate uptake and oleic acid incorporation provides strong evidence that dimethenamid may act upon a primary, specific target in lipid metabolism. Furthermore, the comparable biological activities of dimethenamid and alachlor indicate that this target is common to both N-phenyl and N-thienyl chloroacetamide herbicides. © 1997 SCI. 相似文献
19.
Michael Elliott Andrew W. Farnham Norman F. Janes Diana M. Johnson David A. Pulman 《Pest management science》1987,18(4):223-228
Substituted phenylacetaldehydes, made by homologation of the benzaldehydes by Wittig condensation with a methoxymethylene ylid, were condensed under Wadsworth-Emmons conditions to give the substituted N-(2-methylpropyl)-6-phenylhexa-2,4-dienamides. Electron withdrawing substituents favoured the formation of the unwanted 3,5-diene isomer. Insecticidal activity was lowered by most substituents examined, but was retained or even enhanced by halogen atoms at the m- or p-positions. At the m-position, activity decreased as size of halogen increased. 相似文献
20.
A method is described for the estimation of residues of the carbamate insecticide promacyl [5-methyl-m-cumenyl butyryl(methyl)carbamate] and its metabolites that are hydrolysable to isothymol (m-cymen-5-ol), using high-performance liquid chromatography with electrochemical detection to determine the isothymol. Clean-up of samples relied on the steam volatility of phenols. Recoveries at the 0.1 mg kg?1 level varied from 72–88% for fat tissue and 81–91% for liver. The limits of detection were found to be 0.01 mg kg?1 for and 0.02 mg kg?1 for liver. A comparative study of the chromatography of sample extracts using both ultraviolet detection and electrochemical detection showed a substantial decrease in the level of interfering co-eluates in the latter method. A field trial, involving a single spray application of the formulated acaricide on milking cattle, revealed residues in the butter fat comparable with those found in a previous investigation. 相似文献