共查询到17条相似文献,搜索用时 78 毫秒
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土壤中烟嘧磺隆和莠去津的高残留往往会导致后茬大豆药害问题。本研究建立了一种分散固相萃取-超高效液相色谱-串联质谱法同时检测大豆植株及土壤中烟嘧磺隆、莠去津及其代谢物残留方法。样品经含2%甲酸的乙腈提取, 经分散固相萃取净化, 以乙腈和0.2%甲酸水为流动相, 采用Poroshell 120 EC-C18色谱柱梯度洗脱, 基质匹配标准曲线外标法定量分析。结果表明:在0.01、0.10 mg/kg和1.00 mg/kg添加水平下, 烟嘧磺隆、莠去津及其代谢物的平均回收率为70%~113%, 相对标准偏差为0.3%~11.8%, 目标化合物质量浓度与对应的峰面积之间在0.001~1 mg/kg范围内线性关系良好, 决定系数R2≥0.984 1, 方法的定量限为0.01 mg/kg。该方法简便、快捷、准确, 适用于土壤和幼苗期至鼓粒期大豆植株中烟嘧磺隆、莠去津及其代谢物的检测。本研究为烟嘧磺隆和莠去津的科学使用及后茬作物的安全种植提供有效监测方法。 相似文献
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利用HPLC法对土壤中莠去津的残留动态、淋溶动态进行了研究。结果显示,莠去津以有效成分2.25 kg/hm2和4.50 kg/hm2的剂量施用时,在土壤中的半衰期分别为19.1 d和18.1 d,即其半衰期与莠去津的施用浓度无关,属于典型的一级动力学反应。在120 d的玉米生长期中,土壤中莠去津在不断降解代谢的同时,逐渐向深层土壤中淋溶,多数莠去津持留在表层土壤中。施用莠去津27 d后,高浓度处理小区莠去津的淋溶深度超过30 cm,深度为10~15 cm处的土壤在施用后27 d莠去津的浓度最大。同一土壤深度,莠去津在高浓度处理小区的残留量要远高于低浓度处理小区。这些结果显示,减小莠去津的用量可以减少莠去津在土壤中的移动,表明低剂量施用莠去津是保护地下水免受污染的一种有效措施。影响莠去津的淋溶作用的主要因素包括使用量和土壤的理化特性。 相似文献
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分散固相萃取-超高效液相色谱-串联质谱法同时检测玉米及其土壤中烟嘧磺隆、莠去津及氯氟吡氧乙酸残留 总被引:1,自引:6,他引:1
采用QuEChERS法结合超高效液相色谱-串联质谱法(UPLC-MS/MS)建立了玉米及其土壤中同时检测烟嘧磺隆、莠去津和氯氟吡氧乙酸残留的分析方法。样品采用乙腈(含体积分数为2%的甲酸)提取,基质固相分散净化后,用UPLC-MS/MS外标法检测定量。结果表明:该方法具有灵敏度高、简便、快速等优点;在0.01~1.0 mg/L质量浓度范围内,3种除草剂的仪器响应值与其质量浓度呈良好线性相关,相关系数大于0.990 6;玉米和土壤样品中3种除草剂的添加水平在0.02~0.5 mg/kg时,平均回收率均为78.9%~117.7%,日内相对标准偏差(RSD)均小于11.6%,日间 RSD 均小于13.9%。 3种除草剂在玉米籽粒、玉米植株和土壤中的定量限(LOQ)均小于7.1μg/kg。 相似文献
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Malcolm Glennie-Holmes 《Pest management science》1974,5(3):251-254
A rapid method for the determination of atrazine (2-chloro-6-ethy!amino-4-isopropylamino-l,3,5-triazine) residues in soil is presented. The method, which is particularly suited to laboratory studies of leaching or degradation, has the advantage of rapid throughput as it requires no clean-up steps. Interference by different soil types, however, prevents its use in normal soil residue assays. 相似文献
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超高效液相色谱-串联质谱法同时测定玉米及土壤中烟嘧磺隆和2甲4氯残留 总被引:2,自引:0,他引:2
采用分散固相萃取法进行样品前处理,建立了超高效液相色谱-电喷雾串联四极杆质谱(UPLC-MS/MS)同时快速检测玉米及其土壤中烟嘧磺隆和2甲4氯残留的方法。样品经乙腈-甲酸[V(乙腈):V(甲酸)=99.9:0.1]提取,C18基质固相分散(DSPE)净化后,采用UPLC-MS/MS、多反应监测模式(MRM)检测,外标法定量。结果显示,烟嘧磺隆和2甲4氯进样质量浓度与峰面积间线性关系良好,在0.005~0.1 mg/kg添加水平范围内,烟嘧磺隆和2甲4氯在不同基质中的平均回收率分别为74.6%~98.0%和81.3%~100.1%,相对标准偏差(RSD)分别为1.1%~3.4%和1.7%~10.5%,定量限(LOQ)均为0.005 mg/kg。 相似文献
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莠去津是玉米田应用的优秀除草剂品种,然而由于其在土壤中残留时间长,常对轮作后茬敏感作物造成严重毒害。采用生物修复菌肥做种肥、结合菌肥拌种和叶面喷施方法,研究对玉米后茬旱直播水稻生长发育及药害修复机理,对土壤中莠去津残留量、水稻生长和生理指标、土壤酶活性进行测定。结果表明:颗粒菌肥做种肥+粉剂菌肥拌种+水剂菌肥叶面喷施是莠去津土壤残留毒害修复的最佳方法,土壤中莠去津含量在喷施菌肥后7 d从施用菌肥前的0.9 mg/kg下降到0.1 mg/kg,水稻叶片叶绿素含量显著增加33.74%,超氧化物歧化酶和过氧化物酶酶活性分别显著提高23.39%和92.57%,丙二醛含量则显著降低48.01%;水稻株高、地上部鲜重、干重分别比对照显著增加22.33%、67.51%和74.80%,根系鲜重和干重分别比对照显著增加33.98%和55.43%;土壤磷酸酶、脲酶及纤维素酶含量分别显著增加49.17%、528.65%和35.21%。 相似文献
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采用高效液相色谱-紫外光谱(HPLC-UV)法,研究了烟嘧磺隆在不同含水量土壤中的消解动态,分析了土壤含水量对其消解的影响。土壤样品经V(乙腈)∶V(磷酸盐缓冲溶液)=1∶4提取,采用HPLC-UV法检测不同含水量的土壤中烟嘧磺隆的残留量。结果表明:在0.25~4 mg/L范围内,烟嘧磺隆峰面积与其质量浓度呈良好线性关系,相关系数为0.999 9。在0.05、0.25和1.25 mg/kg 3个添加水平下,烟嘧磺隆的回收率为91%~106%,相对标准偏差(RSD)为5.4%~9.5%。检出限(LOD)为0.012 mg/kg,定量限(LOQ)为0.04 mg/kg。当土壤含水量小于50%时,土壤水分含量变化对烟嘧磺隆消解的影响较小;当含水量大于50%时,烟嘧磺隆消解半衰期呈先增大后减小趋势,其中在含水量为60%和90%的土壤中消解最快,半衰期分别为19.7和18.6 d。 相似文献
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R J Jettner S R Walker J D Churchett F P C Blamey S W Adkins & K Bell 《Weed Research》1999,39(4):287-295
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. 相似文献
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A soil column experiment under outdoor conditions was performed to monitor the fate of 14C-ring-labelled sulcotrione, 2-(2-chloro-4-mesylbenzoyl)cyclohexane-1,3-dione and atrazine, 6-chloro-N2-ethyl-N4-isopropyl-1,3,5-triazine-2,4-diamine, in water leachates and in the ploughed horizon of a sandy loam soil. Two months after treatment, the cumulative amounts of herbicide residues leached from the soil were 14.5% and 7% of the applied radioactivity for sulcotrione and atrazine, respectively. Maximum leachate concentrations for each herbicide were observed during the first month following application: 120 and 95 microg litre(-1) for sulcotrione and atrazine respectively. After 2 weeks, 78% of the sulcotrione and atrazine was extractable from the soil, whereas after two months only 10 and 4%, respectively, could be extracted. The maximum sulcotrione content in the first 10 cm of soil was identical with that of atrazine. For both molecules, the content of non-extractable residues was low, being around 15%. Sulcotrione seems to be more mobile than atrazine but the consequences for water contamination are similar since lower doses are used. 相似文献