作物中1605农药残留量及其代谢物对氧磷的薄层色谱-酶抑制扫描定量分析法

薄层色谱-酶抑制方法对有机磷及氨基甲酸酯类农药的残留量、代谢产物或酶抑制物的分析,其检出量可达毫微克级(10~(-9)克),甚至可达微微克级(10~(-12)克)。     

TLC-EI测定杀虫烟剂残留量的研究

应用TLC-EI(薄层-酶抑制)技术并采用CS-910型仪,对有机磷类及氨基甲酸酯类某些农药混合组成的杀虫烟剂燃烧后的残留量进行测定,结果一般可达ng级.经测定,能把Ⅲ-SMD烟剂中的西维因、马拉硫磷、敌敌畏三种农药分开.色斑可长期保留,Rf值分别为0.710、0.875、0.538.在大气烟雾中的有效烟率分别为4.16％、2.13％、0.76％.3h内松针上最高残留量分别为102.715、19.332、6.701ppm.12h后残渣中农药残留量分别为76、13.42、4.56ppm.用大白鼠肝酯酶测定农药的最小检出量分别为1.21、7.45、0.112ng.     

气相色谱法测定城市自来水中有机氯农药的残留

水中有机氯农药经有机溶剂如环已烷的萃取浓缩后,由高纯氮气载入色谱柱进行分离,载有有机氯农药的氮气进入电子捕获检测器ECD后,其出峰顺序为①α-HCH②γ-HCH③β-HCH④δ-HCH⑤P,P-DDE⑥O,P-DDT⑦P,P-DDD⑧P,P-DDT。用该方法测试的结果表明,在去离子水中添加10ug/L级待测物时,各种待测物的回收率为9350%~9906%(3次平均值),相对标准偏差(RSD)为6%~18%(7次测定平均值)。最低检出量为005ug/L~033ug/L。文中阐述的方法改进了现有的GB5750-85方法中的萃取方法,取得了令人满意的结果。本文也给出了几种常见有机氯农药最小检出量,并在检测水源水的实际工作中得到应用。     

广东省荔枝园土壤农药残留现状研究

荔枝收获完毕后在广东省荔枝主产区采集208个荔枝园土壤样本,检测了9种荔枝常用农药甲霜灵、代森锰锌、多菌灵、溴氰菊酯、氯氰菊酯、三氟氯氰菊酯、敌百虫、乐果和敌敌畏的残留含量.结果表明,农药检出率为氯氰菊酯(59.1%)多菌灵(51.0%)代森锰锌(11.1%)甲霜灵(6.7%)三氟氯氰菊酯(3.4%).乐果和敌敌畏仅在个别果园检出,溴氰菊酯和敌百虫均未检出.土壤同时检出不同种类农药果园的百分数为只检出1种农药(40.4%)同时检出2种(31.3%)未检出(18.8%)同时检出3种(8.2%)同时检出4种(1.4%).检出的7种农药中,代森锰锌残留平均含量最高达39.05μg·kg-1,氯氰菊酯次之为7.83μg·kg-1.其它5种农药平均含量为0.19～1.65μg·kg-1.整体上广东省荔枝园土壤农药残留状况较轻.     

农药残毒速测技术

农药残毒速测技术包括农药残毒速测箱和薄层—植物酶抑制技术两部分。农药残毒速测箱是根据有机磷和氨基甲酸脂农药对胆碱脂酶(ChE)产生抑制作用的机理进行设计和研制的。将ChE与样品提取液反应,若ChE受到抑制,就表明样品提取液中含有机磷或氨基甲酸脂类农药。由于ChE对菊脂类农药不敏感,可以与有机磷或氨基甲酸脂农药相分辨。主要反应式如下:     

我国区域性水体农药污染现状研究分析

以4大流域为基础,较为全面地概述了我国区域性农药污染情况,并对其污染原因进行了分析。结果表明:长江流域有机磷农药、氨基甲酸酯类农药以及部分拟除虫菊酯类农药的的残留量很高;珠江流域农药污染情况较轻,检出量均低于我国地表水环境质量标准;黄淮海流域和松辽流域主要检出农药为酰胺类和三嗪类农药,但具体检出物质存在差异。研究分析表明各流域农药污染与该区域的农作物种类有重要关系。     

间接原子吸收法测定水中可溶性硫化物

水中硫化物常用的测定方法有碘量法及对氨基二甲苯胺比色法。硫化物浓度低于1mg/l时,采用较为灵敏的对氨基二甲苯胺比色法。该法最小检出量为2.5mg。取样50ml时,最低检出浓度为0.05mg/l。     

湘江流域土壤中有机氯农药的残留规律

2004年5月采集了湘江流域51个样品,用AES萃取技术,使用GC-MS方法测定了样品中的六氯苯(HCB)、滴滴涕(DDTs)、氯丹、艾氏剂、狄氏剂、异狄氏剂、七氯和灭蚁灵等有机氯农药(OCPs). 结果表明:HCB和DDTs的检出率为100%,氯丹和灭蚁灵的检出率较低,艾氏剂、狄氏剂、异狄氏剂和七氯未检出,说明HCB和DDTs曾在湘江流域广泛施用. w(OCPs)平均值为145.49 μg/kg,其中w(DDTs)占w(OCPs)的90.9%,且有些土壤样品中w(DDT)/w(DDE+DDD)较大,说明DDTs曾作为湘江流域的主要杀虫剂施用过,并且近期仍然有输入. 农药残留量与农药的施用量成正比,农药施用量高的衡阳地区,其土壤中的农药残留量最高. 不同使用功能的土壤中有机氯农药的残留量不同,表现为旱地中的残留量高于水稻地,蔬菜地中以辣椒地的残留量最高.      

新疆沙雅县不同植物类型农田环境中典型农药残留及其风险评价

为确定沙雅县不同植物类型所在农田环境中典型农药残留特征及潜在的人体健康和生态风险水平,于2020年9月29日采集了沙雅县9个区域的植物、土壤和水体样本共55个,采用气相色谱-质谱联用法对样品中47种典型农药赋存水平进行分析.结果表明,3种环境介质中共检出农药23种,土壤、植物和水体中农药检出范围分别为0~70.58 μg·kg^-1、0~1832.18 μg·kg^-1和0~188.53 μg·L^-1.沙雅县3种环境介质中农药残留水平表现为植物>水体>土壤的特征,从不同植物类型区域农药检出情况来看,位于县中心的P1、P2、P6和P8区域污染最为严重,对应区域中农药负荷水平较高的植物为棉花、核桃、红枣和白杨,且残留值贡献较高的7种农药分别为：六六六、毒死蜱、氯氟氰菊酯、氟胺氰菊酯、甲霜灵、苯醚甲环唑和腐霉利;对成人和儿童通过经口摄入、皮肤接触和呼吸吸入这3种途径暴露在土壤表层的农药中造成的人体健康风险进行评价,结果显示,3种方式中经口摄入作为主要暴露途径,且儿童的风险水平显著大于成年人,但两个年龄段风险水平处于可接受范围内;对蚯蚓在土壤中的生态风险水平进行评估,结果显示沙雅县单个农药对土壤中蚯蚓的潜在生态风险水平较低,联苯菊酯为最大贡献农药;对农药的联合作用进行生态风险评估,结果显示P1、P4、P7和P9区域处于中度风险,其他区域处于低风险等级,因此需限制研究区部分农药的使用.     

我国东南地区饮用水源地多种农药的赋存特征及健康风险评估

为阐明我国东南地区典型饮用水源地农药类微污染物的污染特征及生态风险,检测评估了某省7个水库的苯并咪唑类、酰胺类、三唑类和有机磷类等19类共55种常用农药的检出频率、检出浓度以及每种农药对于绿藻、水蚤和鱼类这3种不同营养级生物的风险商.在分析的55种农药中,多菌灵和乙草胺的检出频率为100%,12种农药的检出频率在80%以上.多菌灵的检出浓度最高(77.7 ng·L^-1),其次是乙草胺(51.6 ng·L^-1).风险评估结果显示,大部分农药在目标区域都处于低风险状态.对于3种生物来说,乙草胺是绿藻的风险主导型农药,而多菌灵是鱼类和水蚤的风险主导型农药.     

20种农药在作物中多残留分析方法的研究

报道了20种有机氯、有机磷和拟除虫菊酯类农药在作物中多残留气相色谱分析方法。9种有机磷农药的最低检测浓度为0.34—22.30ppb,8种有机氯农药为0.13—9.76ppb,3种拟除虫菊酯为1.63—17.00ppb。20种农药在四种作物上的添加回收率大于80％,仅敌敌畏与速灭磷在低浓度(0.05ppm)时,回收率偏低。变异系数都小于10％。     

湖南东部地区稻田土壤中有机氯农药残留及分布

2006年3月,在湖南省东部7个地区的城市近郊和工业区附近稻田中多点采集土壤样品,参照EPA8081A标准方法对样品进行处理和分析,以研究20种有机氯农药残留及分布状况.结果表明:稻田土壤中残留的有机氯农药主要为六六六(HCHs)和滴滴涕(DDTs)类,共占有机氯农药残留总量的84.6%,2种污染物残留量均低于《食用农产品产地土壤环境质量指标》(HJ332-2006)限值,其中,w(HCHs)为1.7～25.3 μg/kg,平均值为18.2 μg/kg;w(DDTs)为10.5～40.4 μg/kg,平均值为23.8 μg/kg.残留水平较高的是β-HCH,DDT和DDE,w(β-HCH),w(DDT)和w(DDE)的平均值分别为12.9,11.4和9.8 μg/kg;其他13种农药也不同程度地被检出.同国内外其他地区同类农田土壤相比,该残留量处于中等水平,表明湖南东部地区稻田土壤中六六六和DDT的残留具有一定的生态风险.      

Study of multiresidue analytical method for organonitrogen and organophosphorus pesticides in soil and water

A gas chromatographic method without derivatization was developed for the residue analysis of 10 organonitrogen and 9 organophosphorus pesticides in soil and water. The samples were blended or shaken with acetone for extraction. The extracts were cleaned up by coagulation, then, re-extracted with three 50 ml portions of dichloromethane. The final residue was detected by gas chromatography equipped with NPD. All of the 19 pesticides were completely separated at a constant temperature. The method described above was applicable to the simultaneous determination of 10 organonitrogen and 9 organophosphorus pesticides .in soil and water with the satisfactory recovery (from 82.42% to 103.57%), coefficient of variance (from 0.17% to 12.57%) and limit of detection (from 0.0006 ppm to 0.058 ppm).     

高效液相色谱串联质谱法测定烟草中有机氮农药残留

用乙腈、水混合液(体积比1:1)提取,提取液经无水硫酸镁和PSA吸附剂处理,经0.45μm滤膜过滤后,以乙腈/水(含5 mmol/L乙酸铵)溶液作流动相,流速200μl/min,采用高效液相色谱-串联质谱法同时测定了烟草中6种有机氮的农药残留量。检测限为0.01～0.10μg/kg,回收率为70%～107%,相对标准偏差不大于8.92%。     

太湖梅梁湾沉积物中有机氯农药的残留现状

采用GC/ECD分析了梅梁湾沉积物中有机氯农药的残留现状.所测样品中有机氯农药总浓度为1.78～64.74ng/g,其中,HCHs、DDTs在几乎所有采样点都有检出,含量分别是0.23～1.81ng/g、1.78～63.08ng/g.HCHs中,α-HCH与γ-HCH残留水平相当,未检出β-HCH.DDTs中p,p'DDE残留水平较高.数据表明有机氯农药中HCHs可能有新的污染源输入,DDTs在多数采样点发生好氧生物降解,与国内不同水体表层沉积物中HCHs、DDTs的含量相比,梅梁湾沉积物中有机氯农药含量较低.     

The profiles of chiral pesticides in peri-urban areas near Yangtze River: Enantioselective distribution characteristics and correlations with surface sediments

Chiral pesticides account for 30% of pesticides. Pesticides are inevitably leached into the groundwater by runoff. At the watershed level, the distribution characteristics of enantiomers in sediments collected from the river network of an agricultural area near the middle and lower reaches of the Yangtze River were tested, and their potential correlations with the physicochemical properties and microbial communities of the sediments were analyzed. The sediment pollution was serious at sites 8 and 9, with their pollution source possibly being agricultural or industrial sewage. Moreover, there were higher cumulative contents of pesticide residues at sites 4, 8, and 9. Specifically, Cycloxaprid was the most detected chiral pesticide in the study area, followed by Dinotefuran and Diclofop-methyl. Additionally, Ethiprole and Difenoconazole had strong enantioselectivity in the study area. Interestingly, the enantiomers of some chiral pesticides, such as Tebuconazole, had completely different distributions at different sites. Pearson correlation analysis showed that sediment catalase and microbial biomass carbon were important factors for enantioselectivity of chiral pesticides. The effect of sediment physicochemical properties on enantioselective distribution was achieved by influencing the microorganisms in the sediment. Furthermore, the enantioselective distribution of Tebuconazole was closely related to the genus Arenimonas. Overall, the enantioselective distribution of most of the chiral pesticides was positively correlated with the prokaryotic microbial community. This study provides empirical support for agricultural non-point source pollution caused by chiral pesticides, and also lays a research foundation for exploring the factors that affect the fate of chiral pesticides in the environment.     

从干剩余污泥中提取蛋白质的试验研究

以上海市松江区某污水处理厂的剩余污泥为原料,采用酸水解法提取干污泥中的蛋白质,考查了固液比、水解温度、水解时间、pH对蛋白质提取效果的影响。试验结果表明,水解的最佳条件为：水解液的pH为1.25;水解温度为118℃;固液比为1∶3.5;水解时间为5.5h。在此基础上,从安全性和营养性两方面考虑,对提取液中重金属和氨基酸...     

广东省典型区域农业土壤中六六六(HCHs)和滴滴涕(DDTs)的残留及其分布特征

2002年10月—2005年11月采集广东省典型区域(汕头市、湛江市、东莞市、惠州市、中山市、珠海市和佛山市顺德区)的农业土壤表层(0～20 cm)样品444个,采用气相色谱方法对土壤中六六六(HCHs)和滴滴涕(DDTs)进行分析,初步揭示广东省农业土壤中有机氯农药的分布及残留情况. 结果表明:HCHs的检出率为95.9%,w(HCHs)为未检出～104.38 ng/g,平均值5.90 ng/g;DDTs的检出率为95.7%,w(DDTs)为未检出～157.75 ng/g,平均值为10.18ng/g. HCHs的4种异构体中,w(β-HCH)最高,平均值为2.96 ng/g,而p,p′-DDE是3种DDTs异构体中含量最高的,平均值为5.09 ng/g. 不同土壤利用类型中,有机氯农药残留总量为水稻田>菜地>香蕉地>旱坡果园地>甘蔗地,汕头市土壤中有机氯农药残留总量明显高于该研究区的其他地方. 与国内外其他地区农业土壤中的DDTs和HCHs含量和我国土壤环境质量标准(GB15618-1995)相比,广东省典型区域污染程度较低.      

Effect of copper on the degradation of pesticides cypermethrin and cyhalothrin

The influence of coexisting copper (Cu) ion on the degradation of pesticides pyrethroid cypermethrin and cyhalothrin in soil and photodegradation in water system were studied.Serial concentrations of the pesticides with the addition of copper ion were spiked in the soil and incubated for a regular period of time,the analysis of the extracts from the soil was carried out using gas chromatography (GC).The photodegradation of pyrethroids in water system was conducted under UV irradiation.The effect of Cu~(2 ) on the pesticides degradation was measured with half life (t_(0.5)) of degradation.It was found that a negative correlation between the degradation of the pyrethroid pesticides in soil and Cu addition was observed.But Cu~(2 ) could accelerate photodegradation of the pyrethroids in water.The t_(0.5) for cyhalothrin extended from 6.7 to 6.8 d while for cypermethrin extended from 8.1 to 10.9 d with the presence of copper ion in soil.As for photodegradation,t_(0.5) for cyhalothrin reduced from 173.3 to 115.5 rain and for cypermethrin from 115.5 to 99.0 min.The results suggested that copper influenced the degradation of the pesticides in soil by affecting the activity of microorganisms.However, it had catalyst tendency for photodegradation in water system.The difference for the degradation efficiency of pyrethroid isomers in soil was also observed.Copper could obviously accelerate the degradation of some special isomers.     

Separation of chlorinated hydrocarbons and organophosphorus, pyrethroid pesticides by silicagel fractionation chromatography and their simultaneous determination by GC-MS

A silicagel fractionation procedure for environmental sample extracts, which separates chlorinated hydrocarbons(CHCs) and organophosphorus, pyrethroid pesticides into two groups for subsequent instrumental analysis, was developed in this study. This method was achieved by optimizing the fraction cut-off volume of elution and different solvents. Using fully activated silica gel and cut-off CHCs collection after 10ml 10% dichloromethane (DCM) in n-hexane passing through the column resulted in satisfactory separation of CHCs and organophosphorus, pyrethroid pesticides. This procedure had a higher reliability for CHCs than for organophosphorus, pyrethroid pesticides, because there is a relatively reliable recovery for CHCs. This approach is less expensive due to reducing sample pre-treatment time and solvent consumption.