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1.
Benomyl, prochloraz or procymidone, applied as an overall plant spray at the openflower stage, effectively suppressed Botrytis cinerea fruit rot, whereas no control was achieved by foliar application only. Fruit rot was prevented using procymidone applied to the soil 12 days before inoculation of the flowers, whereas benomyl or prochloraz gave little or no control, respectively when applied in the same manner. Bioassays, using Penicillium expansum on leaf and flower extracts of strawberry plants growing in soil treated with procymidone, showed the presence of an inhibitory compound with the same RF value on thin-layer chromatography as that of procymidone. Analysis by gas chromatography and identification by gas chromatography—mass spectrometry established that the fungicide procymidone was translocated from the root system of strawberry plants to the leaves and flowers.  相似文献   

2.
Phenmedipham and desmedipham, when injected into a gas chromatograph with N, N, N-trimethylanilinium hydroxide, reacted to give derivatives having good gas chromatographic properties. By this procedure, these two carbamate herbicides yielded N-methylated 3-methoxyphenylcarbamates. Maximum methylation was obtained when the molar ratio of methylating reagent to herbicide was approximately 16: 1. This technique for preparing derivatives provided rapid qualitative and quantitative chromatography of the substances examined, without side-chain decomposition. The derivatives obtained were identified by means of ultraviolet, infrared and mass spectrometric procedures.  相似文献   

3.
Field trial studies have been performed with captan and fenitrothion on cauliflower to propose maximum residue limits and to study the dissipation of the pesticides. Residue levels have been determined at different times following good laboratory practice using gas chromatography with mass spectrometric detection. The behaviour of residue levels of these compounds after household processing has been analysed using gas chromatography with electron capture detection. Seven days after treatment, residue levels of captan could be detected, but not of fenitrothion. The half-lives of dissipation for captan and fenitrothion were calculated as 0.9 and 1.8 days respectively. Washing did not significantly affect the residual amounts of captan and fenitrothion observed in raw vegetables; however, after cooking, captan had degraded completely, whereas residue levels of fenitrothion were not modified significantly.  相似文献   

4.
A sensitive method for the detection and estimation of residues of the molluscicide, niclosamide, in bananas is described. The procedure involves extraction of the molluscicide, purification of the extract by solvent partition and column chromatography, formation of the heptafluorobutyryl derivative of 2-chloro-4-nitroaniline in 99% yield and determination of the derivative by gas—liquid chromatography with electron-capture detection. Recoveries from fortified bananas were 89 and 79% at levels of 0.02 and 0.2 mg kg?1, respectively. The sensitivity of the method was such that 0.6 pg of the pure derivative could be detected, based on twice the background noise level on the chromatograph.  相似文献   

5.
建立了一种测定元胡、浙贝母和白芍3种中药材中嘧霉胺残留的气相色谱分析方法。样品经二氯甲烷提取,液-液分配,柱层析[m(中性氧化铝):m(弗罗里硅土)=3:2]净化,气相色谱-氮磷检测器(GC-NPD)检测,基质匹配外标法定量,同时经气相色谱-串联质谱(GC-MS/MS)验证。结果表明:在0.02~10 mg/L范围内,分别以正己烷和3种空白基质溶液为溶剂配制嘧霉胺的标准工作溶液,峰面积与相应的质量浓度间呈良好的线性关系,R2均大于0.999;在0.01(元胡中为0.02)、0.1和0.5 mg/kg 3个添加水平下,添加回收率为75%~104%,日内相对标准偏差(RSD)为1.3%~10.2%(n=5),日间RSD为1.2%~9.0%(n=3)。分析方法在元胡、浙贝母和白芍中的定量限(LOQ)分别为0.02、0.01和0.01 mg/kg。该方法的灵敏度、准确度及精密度均符合农药残留分析要求,且简单易行,净化效果好,适用于元胡、浙贝母和白芍中嘧霉胺分析。  相似文献   

6.
本文采用反相高效液相色谱法和改进的气相色谱法对仲丁威含量进行了测定,并与CIPAC采用的正相高效液相色谱法测定了进行了比较。结果表明,反相液相色谱法与正相液相色谱法等效,气相色谱法经改进后降低了仲丁威的热分解,三种方法对仲丁威原药及乳油含量的测定结果的相对误差在允许的范围之内。  相似文献   

7.
A rapid, sensitive and specific high-pressure liquid chromatographic method was developed to analyse residues of binapacryl, bupirimate and diflubenzuron on mature foliage and fruit at intervals after application of the compounds to Worcester and Cox apple trees. The three compounds were applied as commercial formulations in trials to compare integrated pest management with routine farm spray-programmes. The identities of the residues were confirmed by a combination of thin-layer chromatography, ultraviolet spectrometry and gas chromatography/mass spectrometry. Only diflubenzuron persisted on foliage until leaf-fall. None of the applied compounds was detectable on harvested fruit, the minimum quantifiable residue levels being 1, 5 and 2.5 μg kg?1 fresh weight for binapacryl, bupirimate and diflubenzuron, respectively.  相似文献   

8.
建立了一种测定西瓜、瓜叶及瓜田土壤中代森锰锌残留的气相色谱顶空法, 采用代森锰锌工作曲线法进行测定并计算, 消除了由于CS2/代森锰锌的质量转换系数不确定所带来的困难。该方法测定准确度较高, 最低检测浓度0. 1 mg/k g, 可较好地应用于代森锰锌残留测定。  相似文献   

9.
A method is described for the analysis of water, soil and crops for residues of the herbicide butachlor. Residues were extracted with acetone + light petroleum distillate. The extracts were concentrated and purified on a chromatographic column containing aluminum oxide, silver–aluminum oxide and Florisil. Finally, they were quantitated by gas chromatography using an electron-capture detector. The detection limits of various samples were between 0.001 and 0.015 mg kg?1. The average recoveries ranged from 79.4 to 104.6%.  相似文献   

10.
A gas chromatographic residue method for use on animal tissues, fat, and milk is presented for the organophosphorus insecticide iodofenphos. The procedure includes the determination of two potential metabolites, iodofenoxon, and 2,5-dichloro-4-iodophenol. The two phosphorus-containing compounds are analysed by means of a flame photometric detector after cleanup including silica gel column and thin-layer chromatography. The substituted phenol is determined separately as the acetylated derivative using an electron capture detector. Some information on the problem of specificity with regard to possible interferences by closely related insecticides or their corresponding phenols is also given.  相似文献   

11.
嘧菌酯在大豆中的残留及消解动态   总被引:3,自引:0,他引:3  
建立了大豆中嘧菌酯残留的气相色谱测定方法,并研究了其在植株和大豆籽粒中的消解动态和最终残留。样品经乙腈提取,弗罗里硅土玻璃层析柱净化,通过气相色谱-电子捕获检测器(GC- ECD)测定。结果表明,在0.025、0.25、2.0 mg/kg 3个添加水平下,嘧菌酯的平均回收率为93.4%~101.1%,相对标准偏差(RSD)为1.2%~7.5%;最小检出量为1×10-12 g,最低检测浓度为0.025 mg/kg。施药剂量为推荐剂量的1.5倍(有效成分337.5 g/hm2)时,嘧菌酯在大豆植株中的半衰期为0.8~3.6 d。在225、337.5 g/hm2剂量下施药3~4次,测得收获期大豆中嘧菌酯的残留量均低于国际食品法典委员会(CAC)规定的最大残留限量(MRL) 0.5 mg/kg。按照推荐剂量225 g/hm2处理,建议我国嘧菌酯在大豆上的MRL值可暂定为0.5 mg/kg,安全间隔期为14 d,施药次数不超过3次。  相似文献   

12.
二硫代氨基甲酸盐类(DTCs)杀菌剂残留分析方法综述   总被引:5,自引:1,他引:4  
综述了二硫代氨基甲酸盐类(DTCs)杀菌剂及其代谢物的残留分析研究现状,并对当前主要的残留分析方法如分光光度法、气相色谱法、液相色谱法及液相色谱-质谱联用技术和毛细管电泳法进行了较为详细的比较、分析,对DTCs类杀菌剂残留分析方法的未来发展进行了展望。衍生化液相色谱法虽然操作步骤较繁琐、耗时长,但结果稳定可靠,并能区分不同结构类型,是目前重点且被广泛采用的方法,而同时测定DTCs类杀菌剂母体及其代谢物的串联质谱方法将是今后进一步研究的热点课题。  相似文献   

13.
The recognition and isolation of toxic metabolites of diazinon by gas, thin-layer, column and high-pressure liquid chromatography is discussed. The possible toxicological significance of these compounds is considered and some preliminary attempts to assess their importance by experiments with microsomal preparations are mentioned.  相似文献   

14.
莠去津在土壤中的残留试验研究   总被引:1,自引:1,他引:0  
本文介绍了莠去津在土壤中的残留消解动态试验及其检测方法和检测结果。  相似文献   

15.
Upon intravenous application of dihydrochlordene dicarboxylic acid-14C to rats, the radioactivity is quickly excreted, and 44% of the excreted radioactivity consists of metabolites. Nine metabolites have been isolated from feces and urine extracts. Three metabolites could be identified by means of authentic samples by thin layer chromatography, gas chromatography, and mass spectrometry: two isomers of dechlorodihydrochlordene-dicarboxylic acid (metabolites I and II, total 22.5%) and dihydrochlordene-dicarboxylic acid-dimethyl-ester (metabolite III, 11.3%).  相似文献   

16.
克百威及其代谢产物残留分析方法研究进展   总被引:1,自引:0,他引:1  
综述了气相色谱法、液相色谱法、分光光度法、电化学法、免疫分析法等分析方法在克百威及其代谢物残留分析中的应用进展。  相似文献   

17.
Recent progress on the separation and identification of organophosphorus and carbamate pesticides is reviewed. Emphasis has been placed on t.l.c. and g.l.c. methods. Newer techniques, including high pressure liquid chromatography and the use of microwave-excited plasmas as detectors for gas chromatography, are discussed.  相似文献   

18.
Atrazine, DDE, and dieldrin were extracted and concentrated from various surface, subsurface, and finished waters using the macroreticular resin method. Organic components in the concentrates from these waters were separated by gas chromatography; the amounts of the three pesticides in the waters ranged from 0.5 to 42,000 parts per trillion by weight. Every major watershed in the State of Iowa revealed some degree of pesticide contamination and seasonal variations were consistent with agricultural runoff models. Atrazine concentrations were highest of the three pesticides, a symptom of its widespread use in the corn belt. DDE also appeared in substantial quantities, providing further evidence of the persistence of DDT and its metabolites. Water from several shallow wells and finished water from many water treatment plants were also contaminated. Current treatment processes do not effectively remove these pesticides.  相似文献   

19.
催熟番茄中的乙烯利残留量及产品品质分析   总被引:4,自引:1,他引:3  
主要研究了不同催熟处理方式和不同处理浓度对番茄果实中乙烯利残留的影响,以及番茄主要成分含量的变化。采用乙烯利田间催熟和浸果催熟两种方式,并选择不同处理浓度,通过顶空气相色谱、液相色谱等分析方法对相关指标进行检测。结果表明,浸果催熟番茄中乙烯利残留量普遍较高,处理浓度在4 000 mg/L时已达1.98 mg/kg,而当处理浓度在6 000 mg/L时,无论是田间催熟或浸果催熟,乙烯利残留量均超出最大允许残留限量(MRL)值(2 mg/kg),分别为2.29、3.14 mg/kg。以2 000 mg/L乙烯利溶液浸果催熟后,番茄中番茄红素、Vc、总糖和可溶性固形物含量分别下降55.6%、13.6%、13.6%和7.1%;而有机酸含量无明显改变。揭示高浓度乙烯利催熟会导致番茄中乙烯利残留量超标,经乙烯利催熟后番茄品质会有所下降。  相似文献   

20.
Retention volumes for polychlorobiphenyls (PCB's) and organochlorine pesticides have been measured on “Florisi”b and silicic acid in various activity states using petroleum spirit eluant. The majority of organochlorine pesticides can be separated from PCB's by column chromatography. The exceptions areheptachlor, aldrin and BHC (apart from the gamma-isomer), and the separation of DDE from PCB's was only achieved with highly active silicic acid. With PCB residues normally found, the separations not secured by column chromatography were obtained by gas chromatography.  相似文献   

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