微波萃取-气相色谱/质谱法测定土壤中的有机氯农药

通过微波萃取提取土壤中的有机氯农药,萃取溶液经浓硫酸脱色、佛罗里硅土柱净化,最后用气相色谱/质谱法分析.以石英砂为基体进行加标回收测定,有机氯农药的回收率在75.5%～103%之间,检出限为0.01μg/kg.  

河流沉积物中有机污染物的分析研究进展

总结了近年来河流沉积物中有机污染物的研究进展 ,集中评述了国内有关沉积物中多环芳烃、有机氯农药和多氯联苯的分析研究现状 ,包括样品采集、样品前处理和样品分析 ,并对今后河流、湖泊及水库沉积物中污染物的分析工作作了展望  

土壤中有机氯农药残留分析前处理方法研究

利用硅胶柱、氟罗里土柱净化前处理方法对浙江某地区土壤样品中六六六、滴滴涕有机氯农药的残留量进行分析,并与现行的GB/T 14550-1993浓硫酸净化前处理方法进行比较。实验结果表明,采用柱净化前处理方法加标回收率在78%～121%,两种前处理方法所得气相色谱分析结果的平均相对标准偏差小于±20%,表明利用柱净化前处理方法能满足痕量有机物残留分析的要求。  

串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯

建立了用加速溶剂萃取仪(ASE)萃取、凝胶渗透色谱(GPC)净化、气相色谱/串联四极杆质谱多反应监测、同时测定土壤中17种有机氯农药和19种多氯联苯的方法.加标浓度在3.3μg/kg时的平均回收率在79.6%～93.2%之间,相对标准偏差在2.9%～13.0%之间,定量限在0.01～0.51μg/kg之间.在检测土壤样品中的有机氯农药和多氯联苯残留方面,Gc-QqQ-MS/MS相对于气相色谱/电子捕获检测器(GC-ECD)和GC-MS的选择离子检测(SIM)模式具有非常明显的优势,尤其是在低浓度水平的定性和定量方面.  

Residues of organochlorine pesticides in water and suspended particulate matter from the Yangtze River catchment of Wuhan, China

The residues of 13 organochlorine pesticides (OCPs) in surface water and HCHs and DDTs in suspended particulate matter (SPM) from rivers and lakes in Yangtze River catchment of Wuhan, China, were investigated. The concentration of total OCPs in surface water varied from 1.01 to 46.49 ng l⁻¹ (mean 10.55 ng l⁻¹). The levels of total HCHs (ΣHCH) and total DDTs (ΣDDT) in surface water were in the range of 0.55–28.07 ng l⁻¹ and lower than detection limit to 16.71 ng l⁻¹, respectively, which was lower than Chinese standards on the whole. For OCPs residues in SPM, the mean levels varying from 0.20 to 34.72 ng l⁻¹ and 0.46 to 2.72 ng l⁻¹ for ΣHCH and ΣDDT, respectively, which ranked the relatively higher levels among Chinese studied rivers. Results from this investigation showed that previous excessive usage of technical OCPs was the main reason for the residues of HCHs and DDTs both in surface water and SPM, although some new sources were likely to occurred in the region. Apart from the OCPs in SPM originated from upstream in flood season, one of the important sources of OCP residues both in water and SPM in Yangtze River was supposed to be the inputs of its tributaries. Additionally, in situ water-SPM phase distributions of OCPs indicated that HCHs tended totransport with water as well as DDTs was prone to combine with SPM in Yangtze River catchment of Wuhan.  

Determination and Assessment of HCHs and DDTs Residues in Sediments from Lake Dongting, China

The contamination of organochlorine pesticides hexachlorocyclohexane (HCH) and Dichlorodiphenyltrichloroethane (DDT) and their eco-environmental assessment in surface sediments from Lake Dongting, the second-largest freshwater lake in China, were studied. Concentrations of ∑HCH (=α-HCH + β-HCH + γ-HCH +δ-HCH) were 0.21--9.59 ng/g dry weight and those of ∑ DDT = p,p'-DDD+p,p'-DDE+o,p'-DDT+p,p'-DDT) ranged from under detectable limit to 10.15 ng/g dry weight. The ratios of α-HCH to γ-HCH were above 7 at most sampling sites while no or a small amount of β-HCH were found at all sites, suggesting the degradation of HCH used in the history and possibly current use of HCH in the region. The low ratios (below 2.0 in most cases) of (p,p'-DDE+p,p'-DDD) to p,p'-DDT and high levels of individual isomers of DDT at some sites also suggested that there have still been fresh inputs of DDT into Lake Dongting. Through the comparison between concentrations of HCH and DDT residues in sediments of Lake Dongting and those from other places in China and also from the results of our eco-environmental assessment, it can be concluded that Lake Dongting is the water body with high contamination of both HCH and DDT in its sediments in comparison with other water bodies in China.  

气相色谱法同时测定地表水中的百菌清、环氧七氯和有机氯农药

用正己烷一次同时萃取地表水中的百菌清、环氧七氯和有机氯农药，萃取液脱水后进气相色谱仪进行测定。当取样体积为500ml时，方法检出限为0．01～0．02μg,／L，标准曲线相关系数大于0．999，方法精密度的相对标准偏差为1．5％-4．0％，加标回收率为81．6％～109．6％。该方法用于实际样品测定，结果令人满意。  

气相色谱法同时分析测定土壤中15种有机氯农药残留

采用石油醚+丙酮(3+1,V/V)作为提取溶剂、硫酸钠溶液与弗罗里藻土净化,气相色谱法同时测定贵州150个土壤背景点15种有机氯农药残留.峰面积与保留时间的精密度分别为1.14～5.15,0.01～0.09;线性关系均在0.99以上;加标回收率为84.3%～127.8%;方法检出限为0.003～0.025ng/g.该方法适用于土壤背景点有机氯农药残留量的分析.  

水磨河流域有机氯农药污染调查及防治对策

在对水磨河流域实地勘察的基础上,用GC-ECD定量测定了乌鲁木齐市水磨河底泥中有机氯农药HCHs和DDTs的含量,以此来了解水磨河有机氯农药污染情况。结果表明,样品中HCHs和DDTs含量分别为0.107~111.690和0.476~66.512ng/g,其检出率为100%,说明该流域已经普遍受到有机氯农药污染。针对目前的污染现状提出相应的治理措施,以减轻水磨河有机氯农药的污染。  

Levels and source of organochlorine pesticides in surface waters of Qiantang River, China

Qiantang River is a typical river used for drinking water source, flowing through agricultural area in east China. Surface water samples at 45 sampling sites from the river were collected and analyzed for 13 organochlorine pesticides (OCPs) during six surveys in 2 years of 2005–2006. Sediments, soils, farmland runoff water and dry/wet deposition of this region were also measured for their OCPs residue in order to know possible source of OCPs contamination. The total OCPs concentrations in surface water were 7.68–615.2 ng/l. β-HCH, δ-HCH, Aldrin, Heptachlor, Heptachlor epoxide are the major OCPs in water. The maximum levels of OCPs in water were found in July, while significantly lower OCP concentrations were measured in January. Significant linear correlation was found between the concentration of HCH and that of total 13 OCPs in water. The measured OCP concentrations in sediments, soils, farmland runoff water and dry/wet deposition are discussed in relation to concentrations and patterns found in the surface water. Comparison of OCP levels in sediments and soils led to conclusion that erosion of soil contribute significantly to the contamination of water. The OCPs dry and wet deposition to water body was estimated to 0.49 and 0.86 ton/year, respectively. The ratio of α/γ-HCH and (DDE+DDD)/∑DDT in environmental matrix indicated there probably existed new OCPs input of lindane and dicofol into the river.