圆盘固相萃取富集-气相色谱法测定地表水中有机氯和有机磷农药

采用环境友好的圆盘固相萃取新技术富集水体中有机氯农药和有机磷农药,分别用微池电子捕获检测器(μECD)和火焰光度检测器(FPD)气相色谱法检测,实现了水中有机氯和有机磷农药残留物的测定。结果表明,16种有机氯农药的平均回收率为64.7%~102%,精密度(RSD,n=6)为2.9%~15%;13种有机磷农药的平均回收率为65.9%~104%,精密度(RSD,n=6)为1.7%~17%。方法快速、灵敏、低污染,可用于水体中多种有机氯农药和有机磷农药的残留分析。     

渤海湾的有机氯农药和多氯联苯

有机氯农药(DDT，BHC)和多氯联苯(PCBs)是人工合成的有机氯化合物。它们的化学性质稳定，在环境中能持久地残留并不易受环境中各种因素的作用而降解，它们在生物体内的累积和生物链中的浓缩已构成对人类和生态系统的潜在危害，早已引起世界各国的关注，并公认为全球性的环境污染物。许多国家的学者对不同海区、各大洋海水、沿岸海水、沉积物以及海洋生物体内的DDT, BHC, PCBs作了广泛深入的调查研究(Elear, 1976; Edwand et al, 1975; Ehrhardt, 1981; Harvey, 1973; Osterroht, 1977;Robert, 1976)。我国对近海海域有机氯农药污染状况作过一些调查，但对多氯联苯未见有过报道。、1980年8月作者在渤海湾采集了26个站位的海水样品，22个站位的沉积物样品和8个毛蚶(Arasubcrenata Lischke)样品，分析了其中DDT, BHC, PCBs的含量水平，并对其在渤海湾中的分布特征作了初步探讨。     

北京郊区农田土壤中HCH残留调查及评价

北京郊区农田分析区的土壤样品中,均有不同程度的各种HCH异构体检出.在所测样品中,HCH异构体平均含量由高到低排序为σ-HCH、β-HCH、γ-HCH、α-HCH,而且在各个样品中γ-HCH都没有占据主导地位,说明在土壤中没有新的HCH进入.与商品HCH进行比较,w(α-HCH)和w(γ-HCH)明显下降,w(β-HCH)和w(σ-HCH)却相对上升了,分析得出异构体之间的降解转化速率由大到小排序为α-HCH、γ-HCH、σ-HCH、β-HCH.初步评价近年没有新的HCH来源污染本区,但仍有一定风险.     

北京市有机氯农药填图与风险评价

采用1个样/km2的密度、1个分析组合样/16km2的方法,对北京市784km2范围内的土壤、大气干湿沉降物、大气颗粒物中HCH、DDT的含量和空间分布特征进行有机氯农药填图.查明2000年北京市地表土壤HCH和DDT的平均含量分别为8.80±11.83ng/g、108.99±301.90ng/g.2006年大气干湿沉降物中HCH和DDT平均含量分别为10.09±9.60ng/g、12.99±13.51ng/g,HCH和DDT的年沉降通量分别为996.57±939.96g/a·km2、1291.53±1342.28g/a·km2.2006年大气颗粒物PM10和PM2.5中的HCH含量分别为0.294±0.205ng/m3和0.217±0.137ng/m3,DDT的平均含量分别为1.037±1.301ng/m3和0.522±0.773ng/m3,显著高于2002-2003年度大气颗粒物中HCH(PM100.01786ng/m3,PM250.01731ng/m3)和DDT(PM100.01672ng/m3,PM2.50.02353ng/m3)的含量,表明北京市或周边地区仍在使用含HCH和DDT化学成分的农药.以2000年北京地表土壤和2006年大气干湿沉降物中HCH和DDT的含量为基础,对2020年土壤中HCH和DDT的时空演变的预测显示,即使干湿沉降物中HCH和DDT的沉降通量每年以5%的速率递减,到2020年土壤中HCH和DDT的环境质量仍不能显著改善,而控制和削减北京及周边地区含HCH和DDT成分农药的使用将是改善北京地表土壤环境质量的关键措施.     

GC—MSD定测土壤中有机磷有机氯农药的残留

研究了土壤中有机磷有机氯农药残留的GC—MSD—SIM测定方法。通过乙腈超声提取,佛罗里硅土净化或直接GC—MSD—SIM方法测定有机氯和有机磷农药残留;采用有机质谱离子选择模式采集数据,简化了样品处理流程。实验数据表明该方法灵敏、快速、准确,方法的精密度为2．7～9．4％,检出限为0．005-0．007μg／g,适用于土壤中的有机磷有机氯农药残留的测定。     

PCBs and OCPs in sediments from Hongfeng Reservoir in Guizhou Province, China

In this research, chlorinated hydrocarbons （polychlorinated biphenyls and organochlorine pesticides） were measured by GC-ECD in sediments from the Hongfeng Reservoir area. The concentrations of total PCBs range from 3.2 to 31.6 ng/g, among which PCB28, PCB52 are the major congeners with the concentrations from 0.5 to 4.6 ng/g, and from 0.4 to 28.1 ng/g, respectively. The concentrations of these pollutants decrease from surface to bottom, while the concentrations at 1-4 cm are lower than at 5-8 cm, suggesting the decline of PCBs input. TOC concentrations of sediment are found in a significant positive correlation with those of PCBs, suggesting that PCBs are mainly adsorbed on organic matter and particles. HCHs and DDTs are the predominant organochlorine pesticides with the concentrations ranging from 1.6 to 8.9 ng/g （average 3.2 ng/g） and 0.9 to 25.7 ng/g （average 7.8 ng/g）, respectively. β-HCH and γ-HCH （lindane） are the predominant HCH isomers from sediments, and p, p＇-DDE and p, p＇-DDT are the predominant DDT isomers. DDT/DDE＋DDD and α-HCH/γ-HCH ratios range from 0.6 to 0.9 and 0.1 to 3.0, respectively, which indicates more use of lindane than technical mixtures of HCHs before, and also suggests changes in HCHs and DDTs in the environment. The high values of β-HCH and p, p＇-DDE also show that atmospheric input is one of the important sources of the Hongfeng Reservoir, because β-HCH and p, p＇-DDE are stable and have low Sw and Pv so that they can be easily transferred over a long range in atmosphere.     

Microwave-assisted extraction of organochlorine pesticides from sediments and determination by gas chromatograph with electron capture detection

A simple and rapid procedure to extract organochlorine pesticides （OCPs） from sediments by means of microwave energy is proposed. Sediment samples were irradiated with microwaves in a closed vessel system while immersed in hexane-acetone （1 ： 1, v/v）. The sample extracts were cleaned up using solid phase extraction with Florisil as adsorbent. Pesticides were eluted with hexane-ethyl acetate （80 ： 20, v/v） and determined by gas chromatographic separation with electron capture detection. Three oven programs were assayed with two different solvent mixtures in order to achieve adequate experimental conditions for the complete extraction of organochlorine pesticides from the matrix. Different variables such as the composition of extraction solvent,     

Heavy metals,polycyclic aromatic hydrocarbons and organochlorine pesticides in the surface sediments of mangrove swamps from coastal sites along the Leizhou Peninsula, South China

Contents of heavy metals, polycyclic aromatic hydrocarbons （PA Hs）, dichlorodiphenyltrichloroethanes （DDTs） and hexachlorcy- clohexanes （HCHs） in surface sediments from mangrove areas of the Leizhou Peninsula were analyzed in July and November 2005. Risk assessment criteria applied by Long E R et al. （1995） and Long E D et al. （1995） （effects range low, ERL; effects range mean, ERM） of chemicals in sediments from the gulf or estuary were used to assess the potential ecological risks of heavy metals, PAHs, DDTs and HCHs to aquatic organisms in the studied area. The results indicated that the average contents of zinc, nickel, chromium, lead, copper, arsenic and mercury were （61.97 ± 55.87）, （59.99 ± 39.01 ）, （47.93 ± 28.37）, （26.64± 13.00） , （23.45 ± 41.96）, （9.32 ± 3.62）, （0.14 ± 0.18） mg/kg in dry weight in the sediment samples col- lected from five studied sites in the Leizhou Peninsula, respectively. Cadmium was not calculated due to its content being below the detection limit （ 〈 0.3 mg,/kg）. The average levels of Cr, Cu, Ni, Pb, Zn and Hg exceed their background values. The average contents of Ni were higher than ERM. The contents of PAHs in the sediments from the five studied sites were （79.78 ± 43.70） ng/g in dry weight, far lower than ERL（4 022 ng/g）. The contents of DDE, DDD and DDTs in the sediments from five studied sites were （2.60 ± 4.68）, （ 17.52 ± 27.25 ）, （27.78 ± 46.64） ng/g in dry weight respectively, clearly higher than ERL, and the average contents of DDT were （7.66 ± 15.93） ng/g in dry weight, much higher than ERM. HCHs could be detected in the sediments only from Gaoqiao sampling site, with the average contents （0.07 ± 0.08） ng/g in dry weight.     

浙江沿岸海域经济贝类中有机氯农药和多氯联苯的残留分布与污染评价

对2006年6月和2007年6月采集于浙江沿岸海域12个站位的5种经济贝类样品,采用气相色谱(GC)方法,进行了有机氯农药(HCHs和DDTs)和多氯联苯(PCBs)残留量的检测,分析了不同种类贝类中HCHs、DDTs和PCBs异构体组分特征,探讨了浙江沿岸海域HCHs、DDTs和PCBs残留分布状况、年际变化趋势和DDTs的来源,并与厦门岛东部等5个主要沿海海域进行了污染物残留量的比较。结果表明:(1)调查区各海域贝类中的HCHs、DDTs和PCBs残留量(湿质量)分别为:(ND~7.86)×10-9,(0.72~281.73)×10-9,(ND~97.95)×10-9;残留量(湿质量)平均值分别为:1.50×10-9,33.65×10-9,19.56×10-9。调查区各海域所有贝类中的HCHs残留量,均符合国家一类生物质量标准,DDTs残留量仅在四角蛤蜊中符合国家一类生物质量标准,在其余4种贝类中仅符合国家二类生物质量标准。DDTs残留量平均值明显高于HCHs和PCBs,因此可以将DDTs视为调查区各海域典型的有机氯污染物。(2)在HCHs和DDTs组分中,分别以-αHCH和P,P-′DDT占优势;在PCBs中,以含4~7个氯原子的PCB占主要优势,调查区部分海域有新的HCHs和DDTs污染源。(3)自2006年6月至2007年6月,HCHs和PCBs残留量总体呈下降趋势,而DDTs残留量则呈上升趋势,不同海域的有机氯残留量有较明显差异。DDTs的污染源与农业生产中三氯杀螨醇的使用有关。(4)与厦门岛东部等5个主要沿海地区相比,浙江沿岸海域经济贝类有机氯污染物中,HCHs残留量仍处于较低水平,DDTs残留量处于中等水平,PCBs残留量则处于较高水平。     

C18固相膜萃取-气相色谱法测定饮用水中12种有机氯农药

利用C18固相萃取膜提取水样，气相色谱法（电子捕获检测器）测定饮用水中12种有机氯农药。对洗脱液、水样pH值、萃取压力等条件进行了优化选择，并与液-液萃取做了比较。结果表明，与液-液萃取相比，固相膜萃取具有操作简单、富集倍数高、节省溶剂和耗时短等优点，是萃取水中有机氯农药的有效方法。12种有机氯农药的回收率为85．97％～127．7％，相对标准偏差（RSD，n=5）为4．74％～12．2％，方法检出限为0．014～0．047μg/L。