光化学荧光分析法测定水样中的甲嘧磺隆

用紫外线照射不具荧光特性的甲嘧磺隆,通过生成具有荧光特性的衍生物,研究了甲嘧磺隆在不同介质——水、二甲基亚砜、甲醇,以及在十二烷基苯磺酸钠、十六烷基三甲基氯化铵(CTAC)胶体分散体系中的荧光特性,并对包括溶剂体系、pH值和照射时间在内的影响分析方法灵敏度的物理化学参数进行了优化,建立了在CTAC胶体分散体系中测定水样中甲嘧磺隆的光化学荧光分析(PCF)法。结果表明:在浓度为2×10-3 mol/L 、pH值为9的CTAC胶体分散体系中,用紫外线照射150 s是PCF法测定甲嘧磺隆的最佳条件,此条件下的检测限(LOD)为7 μ g/L,相对标准偏差(RSD)为1.3%;对自然水体样品中甲嘧磺隆的平均回收率为96.9% ±2.2%。所建立的PCF法可有效测定水中残留的低剂量甲嘧磺隆。     

大豆田土壤中氯嘧磺隆残留动态研究

采用高效液相色谱法对大豆田土壤中的氯嘧磺隆残留动态进行了研究。结果表明,氯嘧磺隆在大豆田土壤中的降解半衰期为7～10d,施药后60d其残留量为0．004mg／kg。     

单嘧磺隆在土壤中的残留分析和消解动态研究

研究了新磺酰脲除草剂单嘧磺隆在土壤中的残留分析方法及其土壤消解动态和最终残留。土壤经甲醇和稀氨水混合液提取 ,液液分配及 C18净化 ,浓缩后用带紫外检测器的高效液相色谱仪进行测定。单嘧磺隆的最低检出量为 4 ng,在土壤中的最低检出浓度为0 .0 2 mg/ kg。本方法的添加回收率为 95.10 %～ 10 3.77% ,变异系数为 1.4 7%～ 11.80 % ,符合农药残留分析的要求。运用上述方法 ,测定了单嘧磺隆在北京和山东土壤中的消解动态以及最终残留。结果表明 :单嘧磺隆在土壤中消解的速度较慢 ,在北京土壤中的半衰期为 9.2 4 d,山东土壤中的半衰期为 13.59d。按推荐剂量施药 ,小麦收获时 ,在北京和山东两地土壤中均未检出单嘧磺隆。     

砜嘧磺隆对玉米田杂草的作用与安全性测定

系统测定了25%砜嘧磺隆DF5种用量与38%莠去津SC混用后,对玉米田杂草的作用过程、除草效果、玉米药害症状与变化过程。同烟嘧磺隆进行了比较,提出了适宜用量,可根据当地实际情况用于生产。     

苯磺隆·甲磺隆·氯磺隆混合物的液相色谱分析

本文以甲醇 水 冰乙酸为流动相，采用C18不锈钢柱，检测波长240nm，对苯磺隆、甲磺隆、氯磺隆混合物进行反相高效液相色谱定量分析。该方法的标准差别分别为0.081、0.013和0.013，变异系数为0.886%、0.268%和0.256%，回收率为99.39%、99.29%和99.28%，线性相关系数为苯磺隆r=0.9994、甲磺隆r=0.9992、氯磺隆r=0.9991，线性方程为苯磺隆y=1360088.17x 1389384、甲磺隆y=972186.69X-21262.8、氯磺隆y=789773.50X 86258.8。     

绿磺隆在土壤中的放射性同位素残留分析

本文综述了利用同位素元踪法研究^14C-绿磺隆在土壤中的吸附、淋溶、迁移和降解等特性，分析了^14C－绿磺隆在土壤中的残留动态。     

砜嘧磺隆水分散粒剂防除马铃薯田杂草效果研究

25%砜嘧磺隆水分散粒剂对马铃薯田一年生杂草具有较好的防除效果,尤其对阔叶杂草防效优秀。使用量75～175 g/hm2范围内对马铃薯安全。推荐使用剂量为87.5～100 g/hm2,适宜施药时期为马铃薯3～5叶期,杂草2～3叶期。     

砜嘧磺隆水分散粒剂防除玉米田杂草的效果

25％砜嘧磺隆水分散粒剂对玉米田稗草、马唐、青葙、鸭趾草等都有较好的防效。使用量90g/hm^2和105g／hm^2药后28d对杂草株防效分别为88．0％和89．7％,鲜重防效分别为89．6％和91．3％,且对玉米安全性好,增产效果显著。     

有关砜嘧磺隆市场及产业链分析(2020)

砜嘧磺隆是美国杜邦公司开发的磺酰脲类除草剂,产品兼具高选择性、高效、低毒等优点,是一种重要的玉米田选择性除草剂.2020年全球磺酰脲类除草剂市场规模将达22.73亿美元,使用量可达1.1万吨(折纯).近七年此类产品全球市场规模逐步下滑,而应用量出现小幅增加的态势,并且产品利润普遍变窄,产品竞争加剧.2019年全球砜嘧磺...     

氯嘧磺隆抗体制备的研究

以合成的半抗原与牛血清白蛋白(BSA)的联结物为免疫抗原,获得对氯嘧磺隆高亲合力的兔抗血清,建立了氯嘧磺隆的直接竞争酶联免疫检测方法。抗血清效价为6.4×104,IC50值为10.9 ng/mL,测定的线性范围是0.4 ~295.4 ng/mL。在河水中的添加回收率为87.9% ~115.7%。结构相似的常用磺酰脲类除草剂与氯嘧磺隆抗体的交叉反应率为0.1% ~4.8%。所建立的方法可用于河水中氯嘧磺隆的残留检测。     

Plant sensitivity to atrazine and chlorsulfuron residues in a soil-free system

The sensitivity of 22 major crops, pastures and weeds from the north-east grain region of Australia to atrazine and chlorsulfuron residues was determined in a glasshouse using a soil-free bioassay system. A logistic equation was fitted to the seedling fresh weights as a function of the logarithm of herbicide concentration by non-linear regression and used to calculate the doses for 10%, 30% and 50% inhibition of seedling growth (ID₁₀, ID₃₀ and ID₅₀). The ID₅₀ for atrazine ranged from 0.03 to 0.04 mg a.i. L^–1 for Salvia reflexa Hornem. and barley to 1.47 mg a.i. L^–1 for sorghum. The ID₅₀ for chlorsulfuron ranged from 0.19 to 0.21 μg a.i. L^–1 for lucerne and snail medic to 102 μg a.i. L^–1 for wheat. Based on ID₅₀ values measured, the predicted responses of each species to a range of concentrations of atrazine and chlorsulfuron were classified into four categories ranging from no damage to severe damage. These sensitivity data will assist in planning cropping sequences in soils previously treated with atrazine or chlorsulfuron.     

Determination of N-(3-ethylsulfonyl-2-pyridinyl)-4,6-dimethoxy-2-pyridineamine in soil after treatment with rimsulfuron

An analytical procedure to detect N-(3-ethylsulfonyl-2-pyridinyl)-4,6-dimethoxy-2-pyridineamine, a degradation product deriving from the hydrolysis of rimsulfuron in soil, has been developed. The analytical standard was prepared by basic hydrolysis of rimsulfuron at pH 9 and purification on a silica gel chromatographic column. The compound obtained was stable at high temperature, thus enabling determination by gas chromatographic analysis. Soil samples were extracted with acetonitrile, purified with a SPE C18 cartridge and analysed using both nitrogen phosphorus (NPD) and mass spectrometer detectors. The analytical procedure described proved to be sensitive and reproducible. Recoveries varied from 84 to 90%. The limit of sensitivity was 0·001 mg kg^-1. © 1997 SCI.     

超高效液相色谱法测定吡蚜酮在棉花和土壤中的残留

建立了超高效液相色谱-亲水色谱柱测定吡蚜酮在棉花和土壤中残留量的分析方法。样本在弱碱条件下采用分散固相萃取(QuEChERS)法进行前处理。结果表明:吡蚜酮在棉叶和棉籽中添加水平为0.05~0.50 mg/kg时,其平均回收率分别为76.9%~91.1%和76.4%~93.7%,相对标准偏差(RSD)为7.2%~8.2%和6.2%~9.8%;在土壤中添加水平为0.02~0.5 mg/kg时,平均回收率为83.8%~94.6%,RSD为5.3%~8.0%。在山东和河南两地按推荐剂量(有效成分30 g/hm2)和1.5倍推荐剂量(有效成分45 g/hm2)施用10%吡蚜酮·高效氯氟氰菊酯悬浮剂后4 d,吡蚜酮在土壤和棉叶中的残留量分别低于0.02和0.05 mg/kg;至收获时,其在土壤和棉籽中的最终残留量低于0.02和0.05 mg/kg。     

高效液相色谱法测定甘蔗及土壤中环嗪酮的残留量

建立了高效液相色谱法(HPLC)测定甘蔗及土壤中环嗪酮残留量的方法。甘蔗样品以氯仿提取,经中性氧化铝柱层析净化,HPLC法测定;土壤样品以乙酸乙酯-甲醇(体积比9∶ 1)混合溶剂提取,HPLC法测定;甘蔗和土壤中环嗪酮的最低检测浓度(LOQ)分别为0.02 mg/kg 和0.04 mg/kg;在0.04~0.4 mg/kg添加水平内,土壤中环嗪酮的回收率为79.4% ~86.1%;在0.02~0.5 mg/kg添加水平内,甘蔗中环嗪酮的回收率为84.1% ~95.7%;相对标准偏差均低于6.1%。     

Degradation of the sulfonylurea herbicides chlorsulfuron and triasulfuron in a high-organic-matter volcanic soil

The degradation rates of two sulfonylurea herbicides, chlorsulfuron and triasulfuron, were determined at two application rates, 15 and 30 g a.i. ha^–1, in a sandy loam soil of volcanic origin under controlled environment and field conditions. Residues were measured using a modified gas chromatographic (gc) determination method. Both herbicides degraded rapidly in the acidic soil (pH 5.7) with high organic matter levels (7.3% o.m.), generally according to first-order rate kinetics. The respective half-lives ranged from 22 to 38 d for chlorsulfuron and from 31 to 44 d for triasulfuron under five controlled temperature/soil moisture regimens, ranging from 10 to 30 °C and between 40% and 80% maximum water-holding capacity. Half-lives in the field were considerably shorter (13 d for chlorsulfuron and 12–13 d for triasulfuron). The degradation rates of the herbicides were influenced more by soil temperature than by soil moisture content. Bioassays using white mustard ( Sinapis alba L.) and forage sorghum [ Sorghum bicolor (L.) Moench] were also used to determine the persistence of phytotoxic residues of both herbicides in the field, and the results showed that the effects of chlorsulfuron disappeared within 8 weeks. Triasulfuron residues disappeared within 9 and 14 weeks for the 15 and 30 g a.i. ha^–1 rates respectively.     

西北春小麦和麦田土壤中15种常用农药残留的检测

为掌握西北春小麦和麦田土壤的农药残留污染状况,在调研和总结分析了西北春小麦的病、虫、草害发生和防治措施基础上,采集了我国西北地区甘肃、青海、宁夏的9个春小麦产区的小麦籽粒和麦田土壤样品。针对春小麦病虫草害防治中常用的农药,使用HPLC-MS/MS和GC-MS方法,测定了吡虫啉、高效氯氰菊酯、辛硫磷、毒死蜱等4种杀虫剂,三唑酮及其代谢物三唑醇、戊唑醇、多菌灵、三环唑、苯醚甲环唑等6种杀菌剂,精噁唑禾草灵、苯磺隆、2,4-滴丁酯、炔草酯及其代谢物炔草酸等5种除草剂,共15种农药及代谢物在小麦籽粒和麦田土壤中的残留量。通过与小麦中农药残留限量相比较,评价了西北春小麦的食品安全。结果显示,仅在采自甘肃金昌的小麦籽粒样品中检出了戊唑醇,且未超过最大残留限量,在其他样品中均未检出15种农药的残留,表明西北春小麦和麦田土壤的农药安全性均较高。本研究为掌握小麦籽粒的农药残留和麦田土壤的农药污染情况提供了研究数据,为进一步指导西北春小麦的绿色无公害病虫害防治提供了参考。     

气相色谱-质谱法测定烟叶和土壤中丁硫克百威及其代谢产物的残留

建立了气相色谱-质谱法同时检测烟叶和土壤中丁硫克百威及其代谢产物(克百威和3-羟基克百威)残留量的分析方法。土壤样品用丙酮-石油醚[V(丙酮)∶V(石油醚)=1∶4]混合溶液提取,无需净化;鲜烟叶样品用丙酮-乙腈[V(丙酮)∶V(乙腈)=1∶9]混合溶液提取;烤后烟叶用乙腈提取。鲜烟叶和烤后烟叶提取液经旋转蒸发浓缩后,用弗罗里硅土柱净化。结果表明:在0.05~1 mg/kg添加水平下,丁硫克百威及其代谢产物的平均回收率在74%~99%之间,相对标准偏差(RSD,n=5)在1.5%~9.2%之间。该方法的前处理相对于萃取过程较简单,其准确度、精密度和灵敏度均符合农药残留分析与检测的技术要求,适合于丁硫克百威及其代谢产物在烟叶和土壤中的残留分析与检测。     

超高效液相色谱法测定土壤中多杀菌素和乙基多杀菌素的残留

建立了土壤中多杀菌素(spinosad)A和D以及乙基多杀菌素(spinetoram)J和L残留量的超高效液相色谱(UPLC)检测方法。土壤样品经乙腈-5%氯化钠溶液-1 mol/L氢氧化钾溶液提取,固相萃取柱净化,UPLC检测,外标法定量。结果表明:土壤中多杀菌素和乙基多杀菌素的定量限分别为0.1和0.05 mg/kg;最小检出量分别为8.0×10-7和2.8×10-7g;在0.1~2 mg/kg添加水平下,多杀菌素在土壤中的平均回收率为89%~96%,相对标准偏差(RSDs)为2.1%~4.9%;在0.05~0.5 mg/kg添加水平下,乙基多杀菌素在土壤中的平均回收率为86%~93%,RSDs为1.2%~8.1%。该方法提取效果好,具有良好的灵敏度、回收率和重复性。     

Photolysis of chlorsulfuron and metsulfuron-methyl in methanol

Photolysis of chlorsulfuron and metsulfuron-methyl was studied in methanol under UV light. Their rates of primary photolysis followed first-order kinetics. The main photoproducts were identified as 2-methoxy-4-methyl-1,3,5-triazin-6-amine, 2-chloro-benzenesulfonamide and methyl 2-(aminosulfonyl)benzoate, which entailed the cleavage of the two N–C ureic bonds. Further photolysis of benzenesulfonamide derivatives involved oxidation of −NH₂, cyclisation with loss of CH₃OH, and scission of the C–S bond A trace of methyl o-mercaptobenzoate was also detected. The corresponding photolysis pathways of chlorsulfuron and metsulfuron-methyl were tentatively proposed. © 1999 Society of Chemical Industry