固相微萃取-气相色谱法测定水中甲拌磷及其代谢产物残留

采用固相微萃取技术富集水样中甲拌磷及其代谢产物残留,并用气相色谱法测定。通过优化试验条件,使该方法在0.05 mg/L~1.00 mg/L范围内线性良好,甲拌磷、甲拌磷亚砜和甲拌磷砜方法检出限分别为0.64μg/L、36.1μg/L、1.8μg/L。用该方法测定无公害种植基地的灌溉水样品,3种农药残留均为未检出,水样的加标回收率为60.4%~85.7%,测定5次结果的RSD为3.4%~8.5%。     

气相色谱-脉冲火焰光度检测器测定痕量有机磷农药

在水样和土壤样中分别加入二氯甲烷和丙酮，用超声波提取水样中敌敌畏、乐果、甲基对硫磷、马拉硫磷、对硫磷等5种有机磷农药和土壤样中甲拌磷、二嗪磷、异稻瘟净、杀螟农、溴硫磷、水胺硫磷、稻丰散、杀扑磷等8种有机磷农药，大大地简化了测定的预处理过程。应用气相色谱法HP—5石英毛细管柱分离，脉冲式火焰光度检测器检测，取得了较好的测定结果。水样中农药的检测限≤0．O02mg／L，土壤样中农药的检测限≤0．O02mg／kg，相对标准偏差水样＜7％，土壤样＜10％，加标回收率水样在84％—96％之间，土壤样在80％—108％之间，均满足测定要求。     

基质固相分散—加速溶剂萃取ASE—气相色谱法测定土壤中毒死蜱残留量

建立了用氧化铝和活性碳作为基质固相分散剂的加速溶剂萃取方法预处理土壤样品中的毒死蜱,用丙酮、甲醇(1∶1,V/V)在加速溶剂萃取仪上以10.3Mpa、60℃提取10 min,萃取液经浓缩定容后,用Agilent 6890气相色谱仪进行检测,土壤中毒死蜱农药的回收率为89.2%～92.8%。该法用于土壤中毒死蜱的农药残留测定,速度快,检出限为0.001 mg/kg。     

大体积进样-气相色谱法测定水中多种痕量有机磷农药

建立了大体积进样气相色谱-火焰光度法检测水中多种痕量有机磷农药的方法.重点研究了程序升温汽化(PTV)进样条件的选择,通过对分流排空量、吹扫时间、PIV起始温度等PTV参数的选择,优化了测试条件,提高了检测灵敏度.水中9种有机磷农药的线性良好,10ml水样中三乙基偶磷硫酯的检出限为0.01μg/L,硫磷嗪、致螟磷、甲拌磷、乐果、乙拌磷、甲基对硫磷、对硫磷和氨磺磷的检出限可达0.001μg/L.水中添加多种有机磷农药准确度精密度试验,平均回收率为85.8%～108%,相对标准差在3.3%～11.4%之间.与常规方法相比,该方法前处理简单快速、分析成本低.灵敏度、准确度和精密度均符合地表水检测质量的要求,适用于水环境中多种农药残留的快速检测.     

骆马湖地区水体、沉积物中农药筛查和分布特征

采用气相色谱/质谱（GC/MS）非靶向筛查技术,分别于2019年11月5—7日（枯水期）、2020年4月24—26日（平水期）和2020年7月15—16日（丰水期）对骆马湖地区水体和沉积物中的农药残留进行了筛查并对其空间分布特征进行研究。结果表明,水中筛查出主要农药13种,除草剂占比62%,检出率＞95%的农药有丁草胺、环嗪酮、异丙甲草胺、多效唑、噻氟菌胺、稻瘟灵、毒死蜱、阿特拉津、避蚊胺和莠灭净,阿特拉津检出质量浓度最高（ND～10 599 ng/L,平均值为725.5 ng/L）,其次为多效唑（ND～2 089 ng/L,平均值为237.0 ng/L）和噻氟菌胺（ND～1 991 ng/L,平均值为237.2 ng/L）。与国内其他地区相比,骆马湖地区水中农药污染处于中等水平,其中阿特拉津、稻瘟灵和毒死蜱的生态风险值得重点关注。骆马湖及入湖河流水中农药总质量浓度呈现丰水期＞平水期＞枯水期的特点,与地表径流、农药的性质及其在水体中的释放等因素有关,丰水期入湖口和省界来水中农药对饮用水水源地的影响较大。沉积物中筛查出9种农药,总体含量不高,且仅扑灭净和避蚊胺检出率>95%,其余<20%。     

江苏省主要农药产品的环境残留监测方法研究

介绍了江苏省生产的主要农药品种，综述了草甘膦、丁草胺、乙草胺、百草枯和氟乐灵等5种除草剂，代森锰锌、戊唑醇、百菌清、甲基硫菌灵和三环唑等5种杀菌剂，毒死蜱、吡虫啉、氯氰菊酯等3种杀虫剂，以及乙烯利、多效唑等2种植物生长调节剂的生产现状及危害，以及上述农药在水、土壤等环境介质中的检测方法。以期为相关农药残留的检测方法标准化、环境中控制限值的制定、农药类环境事故应急监测以及农药生产与使用的环境监管提供技术支持。     

气相色谱法测定土壤中菊酯类农药残留

以正己烷/丙酮混合溶剂(体积比为1∶1)为提取剂,采用Florisil柱净化、气相色谱电子捕获检测器测定土壤中菊酯类农药残留,优化了提取条件。4种菊酯类农药在0.010 mg/L~1.00 mg/L范围内线性良好,方法检出限为0.005 mg/L~0.010 mg/L,甲氰菊酯回收率为85.2%~103%,RSD为2.3%~5.4%;氯氰菊酯回收率为80.5%~103%,RSD为2.8%~6.7%;氰戊菊酯回收率为80.2%~103%,RSD为2.3%~6.0%;溴氰菊酯回收率为80.8%~103%,RSD为2.4%~6.2%。     

毒死蜱生态毒理与风险研究综述

毒死蜱被认为是一种高效、安全和广谱的含氮杂环类杀虫杀螨剂,被广泛应用于农业生产病虫害的防治中。在中国,毒死蜱曾被列为取代高毒农药的重要品种,并被农业部推荐用于无公害农产品生产的专用杀虫杀螨剂。近年来,由于不断发现的毒死蜱生物毒性及其产生的环境安全问题,美国和欧盟国家已经在某些范围内禁用毒死蜱。综合近几年文献,从环境介质含量、转化行为、生物活性检测以及国外水质基准等方面,对其分别叙述,旨在为今后中国地区毒死蜱的环境健康风险评价、生态风险评价和水质基准制定提供基本参考依据。     

有机磷农药气相色谱测定中的色谱柱

目前国内常用的有机磷农药有敌敌畏、敌百虫、甲胺磷、乐果、1605、辛硫磷、稻瘟净、马拉硫磷、久效磷、杀螟松、保棉丰、磷胺、亚胺硫磷、速灭磷、乙硫磷及甲拌磷等。为测定环境样品中的农药的残留量,在气相色谱分析中常用的固定液主要有:OV—101、OV—17、OV—210、OV—225、QF—1、SE—30、DC—200、DC—550、PEGA及DEGS等。     

固相萃取-气相色谱法测定水中多种农药类内分泌干扰物

建立了水样中用固相萃取小柱提取和净化、GC-ECD检测、GC-MSD定性证实的农药类内分泌干扰物检测方法,该方法样品提取、浓缩、净化步骤简便,能实现31种目标物同时检测。方法检测限0.05~0.50μg/L。添加回收率69%~101%,相对标准偏差低于10%。选择农药包括有机氯类(如滴滴涕、六六六、三氯杀螨醇、艾氏剂、异狄氏剂、狄氏剂、七氯、硫丹、氯丹等),氨基甲酸酯类(如甲草胺、乙草胺等),除虫菊酯类(如氯氰菊酯、速灭菊酯等)及其它农药(如氟乐灵、除草醚、毒死蜱)。该方法应用到测定某水库的水样,水库中31种农药类内分泌干扰物总浓度为48.8~890 ng/L,平均浓度295 ng/L。     

气相色谱—串联质谱法检测水中苯霜灵、甲霜灵、噁霜灵残留量

建立水中甲霜灵、苯霜灵、噁霜灵农药残留量的气相色谱—串联质谱(GC-MS/MS)的检测分析方法。样品采用乙腈提取、固相萃取(SPE)柱净化。采用GC-MS/MS分析时,三种农药在15 mim内完全分离并流出。添加浓度加标回收率为80.6%~88.4%,相对标准偏差(RSD)小于5.0%。在0.01~0.20 mg/L质量浓度范围之间线性关系良好(r~20.999 0)。该方法的灵敏度、精密度和准确度均满足农药残留分析要求,适用于水中的农药残留的快速筛查与定性、定量分析。     

Impacts of pesticides in a Central California estuary

Recent and past studies have documented the prevalence of pyrethroid and organophosphate pesticides in urban and agricultural watersheds in California. While toxic concentrations of these pesticides have been found in freshwater systems, there has been little research into their impacts in marine receiving waters. Our study investigated pesticide impacts in the Santa Maria River estuary, which provides critical habitat to numerous aquatic, terrestrial, and avian species on the central California coast. Runoff from irrigated agriculture constitutes a significant portion of Santa Maria River flow during most of the year, and a number of studies have documented pesticide occurrence and biological impacts in this watershed. Our study extended into the Santa Maria watershed coastal zone and measured pesticide concentrations throughout the estuary, including the water column and sediments. Biological effects were measured at the organism and community levels. Results of this study suggest the Santa Maria River estuary is impacted by current-use pesticides. The majority of water samples were highly toxic to invertebrates (Ceriodaphnia dubia and Hyalella azteca), and chemistry evidence suggests toxicity was associated with the organophosphate pesticide chlorpyrifos, pyrethroid pesticides, or mixtures of both classes of pesticides. A high percentage of sediment samples were also toxic in this estuary, and sediment toxicity occurred when mixtures of chlorpyrifos and pyrethroid pesticides exceeded established toxicity thresholds. Based on a Relative Benthic Index, Santa Maria estuary stations where benthic macroinvertebrate communities were assessed were degraded. Impacts in the Santa Maria River estuary were likely due to the proximity of this system to Orcutt Creek, the tributary which accounts for most of the flow to the lower Santa Maria River. Water and sediment samples from Orcutt Creek were highly toxic to invertebrates due to mixtures of the same pesticides measured in the estuary. This study suggests that the same pyrethroid and organophosphate pesticides that have been shown to cause water and sediment toxicity in urban and agriculture water bodies throughout California, have the potential to affect estuarine habitats. The results establish baseline data in the Santa Maria River estuary to allow evaluation of ecosystem improvement as management initiatives to reduce pesticide runoff are implemented in this watershed.     

Ambient toxicity due to chlorpyrifos and diazinon in a central California coastal watershed

The Salinas River watershed along the central coast of California, U.S.A., supports rapidly growing urban areas and intensive agricultural operations. The river drains to an estuarine National Wildlife Refuge and a National Marine Sanctuary. The occurrence, spatial patterns, sources and causesof aquatic toxicity in the watershed were investigated by sampling four sites in the main river and four sites in representative tributaries during 15 surveys between September1998 and January 2000. In 96 hr toxicity tests, significant Ceriodaphnia dubia mortality was observed in 11% of the mainriver samples, 87% of the samples from a channel draining anurban/agricultural watershed, 13% of the samples fromchannels conveying agricultural tile drain runoff, and in 100% of the samples from a channel conveying agricultural surface furrow runoff. In six of nine toxicity identificationevaluations (TIEs), the organophosphate pesticides diazinon and/or chlorpyrifos were implicated as causes of observed toxicity, and these compounds were the most probable causes oftoxicity in two of the other three TIEs. Every sample collectedin the watershed that exhibited greater than 50% C. dubia mortality (n = 31) had sufficient diazinon and/or chlorpyrifos concentrations to account for the observed effects.Results are interpreted with respect to potential effects on other ecologically important species.     

Vegetated ditches as a management practice in irrigated alfalfa

The organophosphate (OP) insecticides diazinon and chlorpyrifos have been frequently detected in the San Joaquin River, California, USA. Irrigation tail waters are a significant source of OP pesticides in the watershed. This study tested several management practices for reducing offsite movement of chlorpyrifos to surface water from flood irrigated alfalfa. Management practices evaluated include (1) a constructed, vegetated irrigation tailwater return ditch and (2) increased lag time between chlorpyrifos application and start of flood irrigation. Chlorpyrifos concentrations in whole-water samples of irrigation runoff were variable and ranged from 0.22 mug/l to a maximum of 1.67 mug/l. The median concentration reduction at the end of a 200 m vegetated ditch was 38% compared to 1% in an adjacent conventional tail water ditch. Runoff data collected represented first flush runoff from sets that were irrigated between 48 and 144 h after chlorpyrifos application. There was no consistent effect of irrigation lag time on chlorpyrifos concentration in tailwater for lag times of up to 144 h. Consequently these data indicate that delayed irrigation is not an effective management practice for reducing chlorpyrifos off-site movement to surface water in California flood irrigated alfalfa.     

Pesticide residue level in tea ecosystems of Hill and Dooars regions of West Bengal, India

In the present study we quantified the residues of organophosphorus (e.g. ethion and chlorpyrifos), organochlorine (e.g. heptachlor, dicofol, alpha-endosulfan, beta-endosulfan, endosulfan sulfate) and synthetic pyrethroid (e.g. cypermethrin and deltamethrin) pesticides in made tea, fresh tea leaves, soils and water bodies from selected tea gardens in the Dooars and Hill regions of West Bengal, India during April and November, 2006. The organophosphorus (OP) pesticide residues were detected in 100% substrate samples of made tea, fresh tea leaves and soil in the Dooars region. In the Hill region, 20% to 40% of the substrate samples contained residues of organophosphorus (OP) pesticides. The organochlorine (OC) pesticide residues were detected in 33% to 100% of the substrate samples, excluding the water bodies in the Dooars region and 0% to 40% in the Hill region. The estimated mean totals of studied pesticides were higher in fresh tea leaves than in made tea and soils. The synthetic pyrethroid (SP) pesticide residues could not be detected in the soils of both the regions and in the water bodies of the Dooars. Sixteen percent and 20% of the made tea samples exceeded the MRL level of chlorpyrifos in Dooars and Hill regions respectively. The residues of heptachlor exceeded the MRL in 33% (April) and 100% (November) in the Dooars and 40% (April) and 20% (November) in the Hill region. Based on the study it was revealed that the residues of banned items like heptachlor and chlorpyrifos in made tea may pose health hazards to the consumers.     

Integrated approach for the quality assessment of freshwater resources in a vineyard area (South Portugal)

An integrated chemical and biological approach for the quality assessment of freshwater resources in a vineyard area of the ??Alentejo?? region (South Portugal) is presented. This includes analysis to 11 pesticide compounds and whole toxicity testing on algae and crustaceans. Simazine, terbuthylazine, terbutryn, desethylatrazine and chlorpyrifos were the most frequently detected pesticides in water collected from wells and drainage channels. Mixtures of up to three compounds in different qualitative combinations were also found. The quality standards for individual pesticides (0.1 ??g L^???1) and pesticides-total (0.5 ??g L^???1) were exceeded in some samples. However, their maximum concentrations were lower than the WHO guidelines, the USEPA health advisory values and the environmental quality standards for priority substances applicable to surface water. In five samples, the herbicides terbuthylazine and terbutryn and the insecticide chlorpyrifos did not pass the toxicity exposure ratio (TER) trigger values specified for aquatic organisms (algae, Daphnia and fish). Maximum toxic effects on Daphnia magna (100%) and Pseudokirchneriella subcapitata (82.56%) were determined in groundwater samples, while in surface water, no toxicity was observed. Concerning effects on Heterocypris incongruens in sediment samples collected at the drainage channels, mortality and growth inhibition values were below 38%. Pro-active management of the use of pesticides is recommended for implementing at the farm and catchment level to reduce inputs into ground- and surface water.     

Organochlorine pesticide residue levels in blood serum of inhabitants from Veracruz, Mexico

The objective of the present study was to monitor the levels of organochlorine pesticides HCB; α-, β-, γ-HCH; pp'DDE; op'DDT; and pp'DDT in blood serum of Veracruz, Mexico inhabitants. Organochlorine pesticides were analyzed in 150 blood serum samples that constituted that which remained after clinical analyses, using gas chromatography-electron-capture detection (GC-ECD). The results were expressed as milligrams per kilogram on fat basis and micrograms per liter on wet weight. Only the following pesticides were detected: p,p'-DDE was the major organochlorine component, detected in 100% of samples at mean 15.8 mg/kg and 8.4 μg/L; p,p'-DDT was presented in 41.3.% of monitored samples at mean 3.1 mg/kg and 1.4 μg/L; β-HCH was found in 48.6% of the samples at mean 4.9 mg/kg and 2.7 μg/L; op'DDT was determined to be in only 3.3% of monitored samples at mean 2.7 mg/kg and 1.4 μg/L. The pooled samples divided according to sex showed significant differences of β-HCH and pp'DDE concentrations in females. The samples grouped according to age presented the third tertile as more contaminated in both sexes, indicating age as a positively associated factor with serum organochlorine pesticide levels in Veracruz inhabitants.     

固相萃取-GC/MS法测定水中16种有机氯农药

采用HLB固相萃取柱富集水样,乙酸乙酯溶剂洗脱,加入氘代菲作为内标,利用气相色谱/质谱联用法选择离子模式测定水中16种有机氯农药,优化了固相萃取条件。16种有机氯农药在5.00μg/L~250μg/L范围内线性良好,按1 L水样计算,方法最低检出限为1.4 ng/L~19.4 ng/L,相对标准偏差为3.5%~20.0%,平均加标回收率为44.7%~119%。     

小体积液液萃取-GC/MS法测定地表水中有机磷农药

采用小体积液液萃取-气相色谱/质谱联用法测定地表水中有机磷农药,以1.2 mL正己烷为萃取剂,磷酸三苯酯为内标,对8种目标化合物的富集倍数达156～436.方法在1.00 μg/L～20.0 μg/L范围内线性良好,8种有机磷农药的检出限均为0.2 μg/L,实际水样平行测定的RSD为2.1%～9.7%,平均加标回收率...