3种杀菌剂拌种防治向日葵黑茎病药效试验研究

进行了3种杀菌剂对向日葵黑茎病的拌种药效试验,结果表明,3种药剂拌种后对向日葵出苗安全,不产生药害;各个处理的防效均随着向日葵生育进程的推进而下降,以出苗后35 d防效最为理想,此时2.5%咯菌腈FS 11.25 mL/hm2、2.5%咯菌腈FS 9 mL/hm2和50%多菌灵WP 13.5 g/hm2的防效为71.7%～83.4%,显著高于50%多菌灵WP 9 g/hm2、70%甲基硫菌灵WP 13.5 g/hm2和70%甲基硫菌灵WP 9 g/hm2,经方差分析证明处理间差异达到显著水平。     

介质液液萃取-高效液相色谱法快速测定蜜桃汁中的多菌灵农药残留

建立了一种以支撑介质液液萃取．高效液相色谱法为基础,快速经济测定果汁中多菌灵农药残留的分析方法。以经过特殊工艺处理的硅藻土为介质液液萃取的吸附填料,对苯并咪唑类农药中有代表性的多菌灵样品进行前处理,结合高效液相色谱法进行分析检测。在优化液相检测条件和萃取条件的同时,从添加回收率、精密度、方法定量限等方面对该方法进行了评价与验证。结果表明,使用介质液液萃取的方法萃取蜜桃汁样品中的多菌灵,添加回收率的平均值在94％以上,方法最低检出限为0．014μg/mL,方法定量限为0．04μg／mL。方法具有前处理简单、分析速度快、经济、重复性好、分析时间短等优点,可推广于其它果汁中多菌灵农药残留的检测。     

Determination of Thiophanate-Methyl and Carbendazim in Rapeseed by Solid–Phase Extraction and Ultra–High Performance Chromatography with Photodiode Array Detection

A rapid and reliable ultra-high performance liquid chromatography method using a photodiode array detector with QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation was developed to determine thiophanate-methyl and carbendazim in rapeseed. Samples were extracted with acetonitrile and partitioned with a mixture of NaCl and anhydrous MgSO₄. The cleanup step was performed using dispersive solid-phase extraction with anhydrous MgSO₄ and primary secondary amine. This step was repeated to improve the results. The limits of detection and quantification of thiophanate-methyl and carbendazim in rapeseed were 15 and 50 μg kg^?1, respectively. The recoveries of thiophanate-methyl and carbendazim were from 77.44–100.9%, with relative standard deviations between 2.20% and 6.62%. The method was employed to determine thiophanate-methyl and carbendazim in rapeseed. This study has established a novel method and a safety evaluation system for the analytes in rapeseed.     

40%戊唑醇·多菌灵水悬浮剂的研制

介绍了农药悬浮剂发展、加工及实验理论依据,采用优化组合法对几种阴离子和非离子表面活性剂的复配体系及其它助剂进行了筛选,对40%戊唑醇·多菌灵水悬浮剂的配方进行了研究,并确定了配制方法和最佳配方组成:戊唑醇20%,多菌灵20%,宁乳34#4.8%,脱糖木质素磺酸钠1.2%,增稠剂(黄原胶∶硅酸镁铝质量比为1∶10)3.2%,乙二醇3%,正辛醇0.1%,水47.7%。实验结果表明,用乳化剂34#、分散剂脱糖木质素磺酸钠、复配增稠剂,采用湿法研磨,该产品悬浮率90%以上,热贮[(54±2)℃,14d]分解率小于5%,产品各项指标符合悬浮剂的要求。     

烯唑醇对水稻重要病原菌的毒力测定及复配研究

烯唑醇对稻纹枯病菌、稻瘟病菌和稻曲病菌具有很强的抑制效果,EC50分别为0.033、0.085和0.147μg/ml。烯唑醇与多菌灵以0.5:10、1.0:10、1.5:10、2.0:10和2.5:10五种比例复配,除1.5:10复配剂对稻瘟病菌的抑制有一定的增效作用外,其他复配剂对稻瘟病菌和纹枯病菌的抑制大都表现为相加作用,而对稻曲病菌的抑制则多为拮抗作用。因此,就增效而言,两者复配对上述三种水稻病害的防治意义不大。     

液相色谱法测定40%多·嘧可湿性粉剂

建立了采用高压液相法测定多菌灵·嘧霉胺粉剂的含量方法.该方法的标准偏差分别为0.162、0.058 3,变异系数分别为0.53、0.57,平均回收率分别为98.11%-100.83%、98.51%-100.98%,方法线性关系良好,其相关系数分别为0.999 9、1.     

杀菌剂氟吗啉和多菌灵对蚯蚓的急性毒性

采用自然土和OECD标准人工土研究了氟吗啉和多菌灵对蚯蚓的急性毒性，并对试验过程中蚯蚓的中毒症状和形态、行为变化进行了观察。结果表明，氟吗啉在自然土壤中对蚯蚓的LC50为592．73mg／kg，95％置信区间为562．41～623．80mg／kg；氟吗啉在人工土壤中对蚯蚓的LC50为318．79mg／kg，95％置信区间为181．63-543．79mg／kg。多菌灵在自然土壤中对蚯蚓的LC50为26．53mg／kg，95％置信区间为15．98-42．93mg／kg；多菌灵在人工土壤中对蚯蚓的LC50为5．57mg／kg，95％置信区间为2．48～11．83mg／kg。依据农药对蚯蚓的毒性等级划分标准，氟吗啉在自然土壤和人工土壤中对蚯蚓的毒性均为低毒级；多菌灵在自然土壤中对蚯蚓的毒性为低毒级，而在人工土壤中对蚯蚓的毒性为中毒级。     

小麦中多菌灵残留量的HPLC分析方法研究

建立了小麦籽粒中多菌灵残留量的高效液相色谱测定法。样品以甲醇提取,二氯甲烷萃取净化,以Lichrospher C18柱(粒径5 mm,4.6mm×250 mm)进行分析,流动相(V甲醇∶V水= 50∶50)流速为1 mL/min时,多菌灵保留时间7.237min。本方法最低检测限为15 g/kg,加标回收率为88%~109%,变异系数4.718%~9.242%。     

高效液相色谱-串联质谱法测定人参中的多菌灵残留

在酸性条件下以甲醇提取人参样品中的多菌灵残留,用高效液相色谱-串联质谱法进行检测。以体积分数0.1%的甲酸-甲醇水溶液梯度洗脱,样品的提取方法为固液萃取,流动相为甲醇,体积流量0.2 mL/min,运行时间10 min。质谱采用正离子扫描模式,定性碎片离子是192.10/160.05、192.10/132.06、192.10/105.06,定量碎片离子为192.10/160.05。仪器检出限和方法检出限分别是0.5 pg和0.022 ng/g,相对标准偏差为1.32%～2.29%,回收率为88.23%～95.07%。研究表明该方法的精准度以及灵敏度均达到要求,适用于人参中多菌灵残留的检测。     

A sensitive determination method for carbendazim and thiabendazole in apples by solid-phase microextraction−high performance liquid chromatography with fluorescence detection

A new analytical method for the determination of carbendazim (MBC) and thiabendazole (TBZ) in apples is reported, based on solid-phase microextraction (SPME) coupling HPLC with fluorescence detection. The main SPME and HPLC experimental conditions were optimized. The apples were first blended and centrifuged. Then, an aliquot of the resulting solution was subjected to SPME on a 60 µm polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 35 min at room temperature with the solution being stirred at 1100 rev min^–1. The extracted pesticides on the SPME fibre were desorbed in the mobile phase into the SPME/HPLC interface for HPLC analysis. The method was linear over the range 0.01–1 mg kg^–1 in apples for both MBC and TBZ, with detection limits of 0.005 and 0.003 mg kg^–1 and correlation coefficients of 0.9995 and 0.9998, respectively. The average recoveries for MBC and TBZ were 91.5 and 92.3% with the relative standard deviations (RSD) of 4.7 and 4.1% at the 0.1 mg kg^–1 level, and 94.6 and 96.1% with RSD of 3.3 and 3.8% at the 0.5 mg kg^–1 level, respectively. The method is simple, sensitive, organic solvent-free and is suitable for the determination of MBC and TBZ in apples.