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在农业生产中混合使用多种农药或兽药越来越普遍,但因药剂联合毒性效应的不确定性而对人体健康产生严重威胁。本文基于酶抑制法原理,利用荧光探针 NEN (N-乙基-1,8-萘二甲酰亚胺) 直接检测CYP3A4酶的活性,建立了广谱筛查混合农兽药联合毒性效应的方法,并以常用的30种农兽药及其典型的23种二元和26种三元组合为研究对象,检测了农兽药混合物对CYP3A4酶的联合毒性效应,其中标准质量浓度根据食品安全国家标准规定的农兽药最大残留限量确定。结果表明:3种质量浓度梯度下对CYP3A4酶均具有协同作用的混合农兽药组合有克百威 + 多菌灵、克百威 + 吡虫啉、啶虫脒 + 烯酰吗啉、吡虫啉 + 多菌灵、氯氰菊酯 + 啶虫脒 + 烯酰吗啉、克百威 + 啶虫脒 + 多菌灵、吡虫啉 + 啶虫脒 + 多菌灵、吡虫啉 + 啶虫脒 + 烯酰吗啉、毒死蜱 + 啶虫脒 + 多菌灵和联苯菊酯 + 啶虫脒 + 多菌灵。当单一农兽药对CYP3A4酶活性的抑制率较高时,与其他农兽药混合后联合毒性效应呈拮抗作用,而当单一农兽药对酶活性的抑制率低于2%时,则与其他农兽药混合后联合毒性效应呈现不确定性。农兽药组合在低浓度下对CYP3A4酶的联合毒性往往存在较强的协同作用,但随着浓度的升高,联合毒性效应从协同变为拮抗作用。分析农兽药与CYP3A4酶之间的构效关系可知,含有芳氯基团的数量与对酶活性的抑制程度成正相关,含有3个芳氯及以上基团的农兽药对CYP3A4酶活性的抑制作用最为显著,抑制率在30%以上,如百菌清、毒死蜱、甲基毒死蜱、咪鲜胺等;含有2个芳氯或“强吸电子基团 + 1个芳氯”基团的农兽药,对CYP3A4酶活性的抑制作用较强,抑制率在18%以上,如苯醚甲环唑、哒螨灵和异菌脲等。具有氨基甲酸酯基团的农兽药单独作用于CYP3A4酶毒性较小或几乎没有毒性时,与其他农兽药混合后显示较强的协同作用。本研究建立的检测方法为广谱筛查混合农兽药联合毒性提供了新思路,检测结果可为进一步在细胞和动物水平制订农兽药混剂的风险评估方案提供依据。 相似文献
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多种农药残留经膳食暴露途径进入人体后，其联合毒性的潜在风险通常超过单一农药。为探明农药多残留的联合暴露毒性，采用经典MTT (噻唑蓝) 比色法，测定了阿维菌素、啶虫脒、多菌灵、百菌清、毒死蜱、高效氯氟氰菊酯、咪酰胺和三唑磷8种农药多种组合方式联合暴露下对HepG2人肝癌细胞增殖的抑制活性。结果表明:联合暴露24 h后，不同种类农药组合对HepG2细胞存活率的影响存在较大差异，随着组合农药质量浓度升高，部分组合对HepG2细胞增殖的抑制效应分别呈现S型变化和线性变化。例如，二元组合 (多菌灵+高效氯氟氰菊酯) 在0~10.00 mg/L、三元组合 (多菌灵+阿维菌素+高效氯氟氰菊酯) 在0~24.12 mg/L、四元组合 (三唑磷+高效氯氟氰菊酯+多菌灵+阿维菌素) 在0~47.46 mg/L以及五元组合 (毒死蜱+阿维菌素+啶虫咪+高效氯氟氰菊酯+三唑磷) 在0~62.80 mg/L暴露条件下其抑制效应表现为S型变化，即随着组合农药质量浓度增大，细胞存活率先迅速降低，之后则缓慢降低；二元组合 (多菌灵+百菌清) 在0~8.46 mg/L、三元组合 (毒死蜱+啶虫脒+多菌灵) 在0~39.97 mg/L、四元组合 (多菌灵+高效氯氟氰菊酯+百菌清+阿维菌素) 在0~25.92 mg/L以及六元组合 (啶虫脒+毒死蜱+三唑磷+多菌灵+高效氯氟氰菊酯+阿维菌素) 在0~57.48 mg/L暴露条件下其抑制效应表现为线性变化，即随着组合农药质量浓度升高，细胞存活率呈线性降低。本研究对农产品中农药多残留的体外细胞毒性进行了评估，明确了不同农药多残留组合对HepG2人肝癌细胞增殖的抑制作用剂量-效应关系，可为进一步探索农药多残留的细胞毒性机制和开展食品安全风险评估提供依据。 相似文献
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本文建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定豇豆中啶虫脒、阿维菌素、甲氨基阿维菌素苯甲酸盐、氟啶虫胺腈、灭蝇胺、苯醚甲环唑、吡唑醚菌酯和烯酰吗啉残留量的方法。样品经乙腈提取,采用ACQUITY_UPLCTMBEH C18色谱柱分离,应用UPLC-MS/MS正离子扫描进行定性定量分析。结果表明,在0.01~1μg/mL范围内,8种农药色谱峰面积与浓度均呈线性相关;3个添加水平下,回收率均在90%以上;8种农药在豇豆中的检出限为0.08~1.81μg/kg,定量限为0.024~0.603μg/kg。在实际豇豆样品检测中检测到5种农药残留,本方法灵敏度高、速度快,可为检测豇豆中8种农药残留量提供参考。 相似文献
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以被苯醚甲环唑、多菌灵及烯酰吗啉污染的铁皮石斛为研究对象,采用乙腈提取,固相分散法净化,高效液相色谱-串联质谱仪分析了3种农药在铁皮石斛鲜条及栽培基质中的残留消解动态,并检测了不同水洗时间、不同溶液浓度（氯化钠和碳酸氢钠）条件下农药残留的去除情况,通过响应面方法确定了农药最佳去除方法。结果表明:3种常用农药在不同添加水平下的回收率为78.5%~106%,相对标准偏差（RSD）为0.7%~4.5%,满足农药残留检测要求;田间试验采用推荐剂量和两倍推荐剂量处理,苯醚甲环唑在铁皮石斛鲜条和基质中的半衰期分别为3.8~3.9 d和4.1~5.6 d;多菌灵的半衰期分别为2.6 d和2.8~3.1 d;烯酰吗啉的半衰期分别为2.8~2.9 d和3.6~5.1 d。响应面法结果显示:经质量分数为5.49%的氯化钠和1.27%的碳酸氢钠混合溶液浸泡5 min后再用清水冲洗45 min,残留的苯醚甲环唑去除率最高;用5.34%的氯化钠和1.22%的碳酸氢钠混合溶液浸泡5 min后再用清水冲洗45 min,多菌灵的去除率最高;而用2.07%的氯化钠和0.80%的碳酸氢钠混合溶液浸泡5 min后再用清水冲洗59 min,烯酰吗啉的去除率最高。本研究可为铁皮石斛质量安全评价体系的建立提供基础数据。 相似文献
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4种杀菌剂及其复配剂对番茄灰霉病菌的毒力 总被引：2，自引：0，他引：2
采用菌丝生长速率法测定了咯菌腈、氟啶胺、啶酰菌胺和苯醚甲环唑4种杀菌剂及其两元复配剂对番茄灰霉病菌的毒力。结果显示,咯菌腈、氟啶胺、啶酰菌胺和苯醚甲环唑对番茄灰霉病菌的有效抑制中浓度(EC50)分别为:0.018 0、0.018 1、1.896 8和2.087 4μg/mL。复配剂啶酰菌胺∶苯醚甲环唑1∶5、1∶3和1∶1,咯菌腈∶苯醚甲环唑1∶5增效作用最明显;复配剂咯菌腈∶苯醚甲环唑1∶3,咯菌腈∶氟啶胺1∶3,啶酰菌胺∶咯菌腈5∶1,啶酰菌胺∶苯醚甲环唑3∶1具有增效作用,SR值范围为1.5~4.05,其中以复配剂啶酰菌胺∶苯醚甲环唑1∶5增效作用最好,其SR值为4.05;其余不同配比的各组合复配剂具有相加作用,其SR值范围为0.5~1.46。表明咯菌腈、氟啶胺、啶酰菌胺和苯醚甲环唑4种不同作用机制的杀菌剂可以交替或复配使用,以阻止或延缓灰霉病菌抗药性的进一步加剧,为灰霉病的综合防控和抗药性治理提供理论依据。 相似文献
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QuEChERS-气相色谱-串联质谱法测定黄瓜中10种农药残留 总被引：2，自引：0，他引：2
建立了黄瓜中氟啶虫酰胺、丁苯吗啉、氟吡菌酰胺、氟啶虫胺腈、环酰菌胺、氟吡菌胺、唑嘧菌胺、氟吗啉、烯肟菌酯和烯肟菌胺10种农药残留的QuEChERS-气相色谱-串联质谱检测方法。样品采用QuEChERS方法，经乙腈涡旋振荡提取，无水硫酸镁和氯化钠盐析后，取5 mL提取液，加入含125 mg PSA、900 mg无水MgSO4和25 mg GCB的组合净化剂进行净化，采用Agilent HP-5 MS Ultra Inert色谱柱分离，气相色谱-串联质谱仪多反应监测 (MRM) 模式测定，基质匹配标准曲线外标法定量。结果表明:在检测浓度范围内，10种农药的质量浓度与其对应的峰面积间呈良好线性关系，决定系数均大于0.99；10种农药的平均回收率在76%~105%之间，相对标准偏差在4.0%~12%之间，定量限在0.001~0.05 mg/kg之间。该方法简便、快速、可靠，适用于黄瓜中10种农药残留的快速检测和分析确证。 相似文献
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为明确常见杀虫剂对日本通草蛉各虫态的影响,在室内分别采用浸渍法和喷雾法测定了12种(8类)杀虫剂对日本通草蛉卵、幼虫、蛹和成虫的毒性,并评价了杀虫剂对日本通草蛉的毒性风险。结果表明,高效氯氰菊酯对日本通草蛉为极高风险,毒死蜱、吡虫啉、烯啶虫胺和阿维菌素为高风险,溴氰虫酰胺、啶虫脒和氯虫苯甲酰胺为中等风险,噻嗪酮、吡蚜酮、螺虫乙酯和甲氧虫酰肼为低风险;与其他虫态相比,12种杀虫剂对日本通草蛉蛹的毒性均为最低。在害虫生物防治及综合治理中应尽量选用对日本通草蛉毒性低的杀虫剂,以起到保护天敌的作用。 相似文献
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QuEChERS-高效液相色谱-串联质谱法测定榛子中4种农药的残留 总被引：1，自引：0，他引：1
建立了同时检测榛子中苯醚甲环唑、丙环唑、噻虫嗪和啶虫脒4种农药残留量的QuEChERS-高效液相色谱-串联质谱 (HPLC-MS/MS) 检测方法。榛仁和榛壳分别经正己烷饱和的乙腈和乙腈提取,用弗罗里硅土、石墨化碳黑 (GCB) 和N-丙基乙二胺 (PSA) 净化。C18色谱柱分离,采用电喷雾正离子 (ESI+) 扫描,在多重反应监测 (MRM) 模式下进行质谱分析,外标法定量。结果表明:在0.01～2 mg/kg范围内,苯醚甲环唑、丙环唑、噻虫嗪和啶虫脒4种供试农药的质量浓度与对应的峰面积间呈良好线性关系 (R2 > 0.990 2)。在0.01、0.1和1 mg/kg 3个添加水平下,4 种农药在榛子中的日内平均回收率为79%～111%,相对标准偏差 (RSDs) (n = 5) 为0.6%～6.9%,日间平均回收率为81%～110%,RSDs (n = 15) 为1.1%～8.5%。4种农药的定量限均为0.01 mg/kg。此方法简单、高效,可为榛子等坚果类食品中多种农药残留的同时测定提供参考。 相似文献
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为明确7种种衣剂对菜薹的安全性及对黄曲条跳甲的防控作用,为黄曲条跳甲的有效防控提供技术支持,采用田间试验研究了乙基多杀菌素、Bt、啶虫脒、唑虫酰胺、虫螨腈、高效氯氟氰菊酯+虫螨腈、高效氯氟氰菊酯+啶虫脒等7种药剂对菜薹出苗、株高、鲜重的影响及对黄曲条跳甲的防控作用。结果表明,7种种衣剂对菜薹安全。除高效氯氟氰菊酯+虫螨腈、高效氯氟氰菊酯+啶虫脒外,其他5种药剂对黄曲条跳甲均具有一定的防控效果,以唑虫酰胺防治效果最好,平均防效高于82%,植株受害率较低,小于5%。 相似文献
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BACKGROUND: Environmental pesticides, including insecticides and herbicides, are frequently encountered as mixtures and threaten non‐target organisms in water. Evaluation of the combined toxicity of diverse pesticides with various concentration combinations is important, especially using limited experimental effort. Uniform design (UD) is one optimal experimental technique that can rationally arrange the concentrations of mixture components so that, with a minimum number of experimental runs, the combined toxicity of multiple pesticide mixtures can be evaluated. RESULTS: The concentration compositions of 18 pesticide mixture points designed by UD covered almost all possible concentration ranges of the mixture components on account of the two merits of ‘space filling’ and ‘multiple levels’. The combined toxicities of 18 mixture rays extended by using the fixed‐ratio ray design (FRRD) from 18 UD mixture points were evaluated by concentration addition (CA) and independent action (IA) models. It was found that the concentration–response curves (CRCs) predicted by CA were, on the whole, located between the 95% confidence intervals of the experimental CRCs, which implied that the combined toxicity of the pesticide mixture rays could be evaluated by CA. The CRCs predicted by IA were very similar to those from CA. CONCLUSION: The model developed from the UD mixture rays can effectively simulate mixtures with arbitrary concentration compositions of 15 pesticides. The CA model can accurately evaluate and predict the combined toxicity of the pesticides, which provides a useful tool for risk assessment of a mixture of multiple pesticides in the aquatic environment. Copyright © 2010 Society of Chemical Industry 相似文献
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白僵菌与杀虫剂科学混用是提高白僵菌杀虫效果的有效措施。本文研究了布氏白僵菌菌株NEAU30503孢子与10种常用杀虫剂混合不同时间后对其孢子萌发和菌落生长的影响。结果表明,杀虫剂种类、混合浓度和时间均能影响孢子萌发和菌落生长,但存在较大差异。几乎所有供试杀虫剂随混合浓度的增加,对孢子萌发的抑制作用有增强趋势;高效氯氟氰菊酯、啶虫脒对孢子萌发影响较小,辛硫磷和氧乐果对孢子萌发影响较大。大多数杀虫剂随混合时间延长,对孢子萌发的抑制作用明显增强;而高效氯氟氰菊酯和毒死蜱与孢子混合1和5 d对孢子的萌发没有明显差异。啶虫脒对菌落生长的抑制作用最小,辛硫磷对菌落生长的抑制作用最强。在供试的10种杀虫剂中,啶虫脒和拟除虫菊酯类杀虫剂与NEAU30503相容性较好。研究结果为布氏白僵菌与杀虫剂的合理混用使用提供了依据。 相似文献
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叶菜上农药原始沉积行为受作物形态、农药种类及其剂型、施用方式等多种因素的影响,是评估农药残留的重要指标。以吡虫啉和啶虫脒为目标农药,以菠菜和生菜作为靶标作物,通过农药施用后的原始沉积行为,以及兑水量、叶面积指数和农药剂型对农药沉积的影响,初步揭示了农药原始沉积规律。结果表明：施药后0.5～8 h内其沉积量无显著差异,综合考虑,选择施药后2 h时测定其原始沉积量;两种农药在菠菜和生菜中主要沉积在叶片表面,沉积量占比均在87%以上,在根和土壤中的沉积量较少;农药施药剂量相同而兑水量不同,则原始沉积量存在显著差异,随着兑水量的增加,沉积量逐渐减少;菠菜和生菜中农药沉积量与叶面积指数呈负相关;原始沉积量与剂型也有相关性,在施药剂量相同时,吡虫啉在菠菜、生菜中原始沉积量最高均为可湿性粉剂,沉积量分别为0.66和0.77 mg/kg;啶虫脒在菠菜中原始沉积量最高为乳油和可湿性粉剂,沉积量均为0.65 mg/kg,生菜中原始沉积量最高为可湿性粉剂,沉积量为0.37 mg/kg。研究结果认为,农药剂型、兑水量和叶面积指数均会影响叶菜表面农药原始沉积量,该结果可为叶菜中农药合理安全施用和农药残留管控提供... 相似文献
15.
Mohsen A. El-Guindy Mostafa M. Abdel-Sattar Abdel Rahman M. El-Refai 《Pest management science》1983,14(3):253-260
The ovicidal action of four insecticides and three insect growth regulators, on eggs of various ages of the susceptible (S) strain of Spodoptera littoralis, was investigated. The results revealed that diflubenzuron was the most toxic compound tested on 0-1-day-old eggs, followed by triprene and then methoprene; chlorpyrifos came next in its toxicity, followed by cypermethrin then fenvalerate; methomyl was the least effective. With the progress of embryonic development, 1-2-day-old eggs showed slight tolerance to the action of the pesticides and juvenoids, but apparently resisted the action of diflubenzuron. Eggs 2-3 days old showed increased tolerance to the insecticides and diflubenzuron and, to a lesser extent, to the action of the two juvenoids. A total of 21 insecticide or insect growth regulator-insecticide mixtures, based on their toxicity equivalents (LD25 + LD25), were applied jointly on 0-1-day-old eggs of the S strain. The mixtures which produced high synergism on this stage could be arranged, according to their decreasing order of potentiation, as follows: fenvalerate/diflubenzuron, cypermethrin/triprene, methomyl/methoprene, cypermethrin/methoprene, fenvalerate/ methoprene, cypermethrin/methomyl, cypermethrin/diflubenzuron, fenvalerate/triprene, diflubenzuron/methoprene and methomyl/triprene. The mixtures that produced synergistic effects on 0-1-day-old eggs were also tested against the 1-2 and 2-3-day-oldeggs of the S strain. Theresults indicated that themixtures fenvalerate/diflubenzuron, and cypermethrin with either triprene or diflubenzuron, when tested on 1-2-day-old eggs, produced levels of synergism nearly similar to those achieved on newly deposited eggs. On the other hand, the mixtures cypermethrin/methomyl, and fenvalerate with methoprene or triprene, showed comparatively lower levels of synergism. However, the synergistic action of the mixture cypermethrin/methoprene, previously detected on newly deposited eggs, became an additive effect on 1-2-day-old eggs. Only the mixtures fenvalerate/diflubenzuron, cypermethrin/triprene and fenvalerate/methoprene showed synergism on 2-3-day-old eggs. The mixtures which showed synergistic effects on 0-1-day-old eggs of the S strain were further tested on eggs of various ages of the diflubenzuron-resistant (Rd) strain. As regards 0-1-day-old eggs, only the combinations cypermethrin/triprene, methomyl/methoprene and fenvalerate/methoprene produced additive effects. The mixture cypermethrin/diflubenzuron was still synergistic against newly deposited eggs of the Rd strain, in a manner similar to that indicated with the S strain. Apparent levels of antagonism were shown to the other insecticide-juvenoid mixtures as well as to the diflubenzuron/methoprene combination. The combinations cypermethrin/methomyl and fenvalerate/diflubenzuron had some effect on the freshly deposited eggs of the Rd strain but produced lower levels of potentiation. With the increase in age of the eggs, the mixture cypermethrin/diflubenzuron showed a lower level of synergism on the 1-2 day-old eggs than was observed in younger eggs. The additive effects, previously detected with some of the mixtures on newly deposited eggs became an antagonistic effect for the 1-2-day-old eggs. The eggs at this stage were more able to resist thejoint action of the other mixtures tested. Moreover, with further increase in the age of the eggs, the combination cypermethrin/diflubenzuron produced a lower level of potentiation on 2-3 day-old eggs, followed by fenvalerate/diflubenzuron at an even lower level, while the other mixtures showed various levels of antagonism. 相似文献
16.
Residues of the pesticides chlorpyrifos, dimethoate, cyhalothrin, cypermethrin, fenvalerate, deltamethrin and chlorothalonil in the autumn Chinese cabbage (Brassica chinensis L.) were studied using gas chromatography. The results indicated that the residues were dependent on the frequency and rate of pesticide application and on the weather conditions immediately following spraying. When the Chinese cabbages were treated once at normal rates, the half-lives of the seven pesticides in the vegetable were 4.7, 5.3, 2.9, 3.5, 5.4, 4.3 and 4.0 days respectively. Thus, based on the recommended preharvest intervals, the residual levels of all pesticides were within the national standards. When the Chinese cabbages were treated four times at maximal rates at 5 day intervals, the half-lives of chlorpyrifos, cypermethrin and chlorothalonil in the vegetable were 3.6, 2.9 and 5.9 days respectively, so that, based on the recommended preharvest intervals, the residual levels of chlorpyrifos and chlorothalonil exceeded the national standards for pollution-free vegetables, but the residual level of cypermethrin was within the national standard. Effects of rain on pesticide final residues in plants treated four times were more significant than in those treated once. 相似文献
17.
七种新烟碱类杀虫剂对韭菜迟眼蕈蚊幼虫及蚯蚓的选择毒力 总被引：5，自引：3，他引：2
为筛选出高效安全的韭蛆防治药剂,室内采用胃毒触杀联合毒力法比较了吡虫啉、啶虫脒、噻虫嗪、噻虫胺、呋虫胺、烯啶虫胺、噻虫啉与毒死蜱和高效氯氟氰菊酯等6种对照药剂对韭菜迟眼蕈蚊幼虫的毒力,同时用人工土壤法测定了13种药剂对蚯蚓的急性毒性,并通过盆栽试验验证了其对韭蛆和蚯蚓的选择毒力。结果表明,吡虫啉、噻虫胺、呋虫胺、噻虫啉、噻虫嗪对韭菜迟眼蕈蚊4龄幼虫的毒力明显高于6种对照药剂,对虫酰肼的相对毒力倍数分别为101.6、55.0、32.9、27.2、13.6;13种供试药剂中,除吡虫啉、啶虫脒、噻虫胺、呋虫胺对蚯蚓中等毒性外,其余均为低毒;盆栽试验中,吡虫啉、噻虫嗪、毒死蜱、噻唑膦、高效氯氟氰菊酯的防虫效果和保苗效果均分别高于其它药剂,但其中只有噻虫嗪对蚯蚓没有明显致死作用。 相似文献