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.     

毛细管气相色谱法分析土壤中有机氯农药

不分流毛细管气相色谱法分析土壤中有机氯农药,可解决样品某些干扰问题。６６６与ＤＤＴ各组分的检测限分别为≤０．０００５和≤０．００２ｍｇ／ｋｇ。     

惠州农业土壤、灌溉水和农产品中有机氯农药的残留

用气相色谱法(GC-ECD)对惠州市51个农业土壤样品、12个灌溉水样品和21个农产品样品中的HCHs和DDTs残留量进行了测定.HCHs平均含量分别为土壤1.66μg/kg、灌溉水5.86ng/L、农产品24.74μg/kg;DDTs平均含量分别为土壤4.98μg/kg、灌溉水2.06ng/L、农产品41.72μg/kg,土壤中有机氯农药通过多种方式进入到水体及农产品中.从HCHs和DDTs异构体组成可以看出,环境中绝大多数农药残留是由于历史上使用造成的,个别地区可能还有新的污染输入.同其它地区相比,惠州农业土壤和灌溉水中的有机氯农药残留水平较低,但农产品尤其是蔬菜中DDTs富集程度较高.     

Monitoring and Assessment of Persistent Organochlorine Residues in Sediments from the Daliaohe River Watershed, Northeast of China

Surface sediment samples from 12 sites of the three selected rivers in Daliaohe River watershed (Hunhe River, Taizihe River and Daliaohe River) were analyzed with the objective of establishing sources and hazard of the organochlorinae pesticides (OCPs) and polychlorinated biphenyl (PCBs) in surface sediments. The total concentrations of OCPs varied from 3.06 to 23.24 ng g⁻¹. ∑HCH (α-HCH, β-HCH, δ-HCH, γ-HCH), ∑DDT (p, p′-DDE, p, p′-DDD, o, p′-DDT, p, p′-DDT) and ∑Cyclodiene (Heptachlor, Aldrin, Heptachlor epoxide, Dieldrin, Endrin) ranged from 1.86 to 21.48, 0.5 to 2.81 and 0.56 to 1.53 ng g⁻¹, respectively. Results of OCPs also illustrate that the most dominant pollutants among the OCPs was ∑HCH, and γ-HCH was the most dominant isomer in HCH, which was evidence of recent input of lindane. It possibly came from the runoff of polluted soils and long-scale transportation. Total PCB concentrations ranged between 1.88 and 16.88 ng g⁻¹. The peak concentrations of PCBs were found in sediments from station T5 and D3, which are in the vicinity of industrial areas and ferry, respectively. These data show a moderate level of OCPs and PCBs contaminations compared to that in other countries.     

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.     

QuEChERS-GC/ECD法分析土壤和沉积物中残留有机氯农药和多氯联苯

建立了用快速、简单、廉价、有效、可靠及安全(Qu ECh ERS)的方法净化、GC/ECD法测定沉积物中有机氯农药和多氯联苯的分析方法。目标化合物质量浓度在1.0~100μg/L范围内线性良好,相关系数均0.999,检出限为0.08~0.17μg/L。以沉积物标准样品SRM1944为研究对象,用Qu ECh ERS方法和传统方法进行提取比较,并用沉积物样品进行验证,回收率为87.8%~100.3%。方法快速、简单、可靠、安全。     

Pesticide Residues in Bovine Milk from a Predominantly Agricultural State of Haryana, India

One hundred forty seven samples of bovine milk were collected from 14 districts of Haryana, India during December 1998–February 1999 and analysed for the presence of organochlorine pesticide (OCPs) residues. ∑HCH, ∑DDT, ∑endosulfan and aldrin were detected in 100%, 97%, 43% and 12% samples and with mean values of 0.0292, 0.0367, 0.0022 and 0.0036 μg/ml, respectively. Eight percent samples exceeded the maximum residue limit (MRL) of 0.10 mg/kg as recommended by WHO for ∑HCH, 4% samples of 0.05 mg/kg for α-HCH, 5% samples of 0.01 mg/kg for γ-HCH, 26% samples of 0.02 mg/kg for β-HCH as recommended by PFAA and 24% samples of 0.05 mg/kg as recommended by FAO for ∑DDT. Concentrations of β-HCH and p,p′-DDE were more as compared to other isomers and metabolites of HCH and DDT.     

加速溶剂萃取-气相色谱质谱法同时测定土壤及沉积物中34种有机氯农药及18种多氯联苯类化合物

建立了加速溶剂萃取-气相色谱质谱法同时测定34种有机氯农药(OCPs)和18种多氯联苯类化合物(PCBs)的方法。当取样量为10. 0 g时,52种有机化合物的检出限为0. 03～0. 29μg/kg,以空白样品为基体进行加标回收试验,平均回收率为44. 7%～123. 0%,相对标准偏差(RSD,n=7)为1. 8%～21. 5%。该方法灵敏度高,实现了低浓度有机化合物的定量分析,分析结果准确可靠,满足土壤和沉积物中34种有机氯农药和18种多氯联苯类化合物分析的要求。     

Organochlorine pesticide residues in ground water of Thiruvallur district, India

Modern agriculture practices reveal an increase in use of pesticides and fertilizers to meet the food demand of increasing population which results in contamination of the environment. In India crop production increased to 100% but the cropping area has increased marginally by 20%. Pesticides have played a major role in achieving the maximum crop production, but maximum usage and accumulation of pesticide residues was highly detrimental to aquatic and other ecosystem. The present study was chosen to know the level of organochlorines contamination in ground water of Thiruvallur district, Tamil Nadu, India. The samples were highly contaminated with DDT, HCH, endosulfan and their derivatives. Among the HCH derivatives, Gamma HCH residues was found maximum of 9.8 μg/l in Arumbakkam open wells. Concentrations of pp-DDT and op-DDT were 14.3 μg/l and 0.8 μg/l. The maximum residue (15.9 μg/l) of endosulfan sulfate was recorded in Kandigai village bore well. The study showed that the ground water samples were highly contaminated with organochlorine residues.     

UPLC-串联质谱法快速测定地表水中多种农药残留

采用超高效液相色谱-串联质谱法测定地表水中21种氨基甲酸酯和有机磷农药,通过优化试验条件,使方法在0. 500μg/L～100μg/L范围内线性良好,方法检出限为0. 1μg/L～6. 2μg/L。对空白水样做3个质量浓度水平的加标回收试验,5次测定结果的RSD为0. 3%～9. 5%,回收率为82. 0%～113%。将该方法用于测定徐州某地表水样品,3个水样均为未检出。     

QuEChERS-气相色谱法快速测定土壤中8种有机氯农药

建立QuEChERS-气相色谱法同时检测土壤中8种有机氯农药的方法,优化分散固相萃取剂用量。土壤样品通过分散固相萃取净化技术,氮吹浓缩后用正己烷定容,最后通过气相色谱测定。结果表明,在2.0~100μg/L质量浓度范围内呈线性,相关系数r为0.9895~0.9991。空白样品在0.5,5和20μg/kg加标浓度下的回收率为75.3%~92.3%,相对标准偏差为3.2%~5.6%(n=5),方法检出限为0.053~0.064μg/kg,测定下限为0.21~0.26μg/kg。该方法操作简单、结果准确、有机试剂用量少、分析成本低,适用于土壤中有机氯农药的残留检测与分析。     

Organochlorine Pesticide Residues in Milk and Blood of Women from Anupgarh, Rajasthan, India

Anupgarh is the most fertile area of Rajasthan state where a variety of seasonal crops are grown. The availability of three manmade canals has enhanced the agricultural activities in this area. The farmers use huge amounts of pesticides to increase the crop productivity. Exposure of humans to these hazardous chemicals occurs directly in the fields and indirectly due to consumption of contaminated diet, or by inhalation or by dermal contact. The organochlorine pesticides are reported to be lipophilic and their presence in human milk and blood has been documented in different parts of the world. Blood and milk samples were collected from lactating women who were divided into four groups on the basis of different living standards viz residence area, dietary habits, working conditions and addiction to tobacco. The level of total organochlorine pesticides in blood ranged from 3.319mg/L—6.253mg/L while in milk samples it ranged from 3.209Mdash;4.608 mg/L. The results are in concurrence with the reports from other countries.     

红壤丘陵区典型流域地表水水环境特征研究——以浏阳河流域为例

选取浏阳河流域为例,根据近十年河流断面监测数据,采用改进的综合污染指数法来评价水质污染程度,研究了该红壤丘陵区典型河流水质的时空变化特征,并结合土地利用和土壤特征等分析地表水质变化原因。结果表明,改进的综合污染指数法有较好的适用性;从时间特征上看,由于面源污染加剧,使得浏阳河近十年的水质污染呈增长趋势;从空间特征上看,浏阳河从上游到下游,河流污染呈增长趋势,上游水质较好,中游表现为重金属铅和汞的污染较大,而下游则是氨氮污染加剧。     

固相萃取-气质联用法测定水中有机氯农药和氯苯类化合物

采用固相萃取-气相色谱-质谱法(SPE-GC-MS)同时测定水中26种有机氯农药和8种氯苯类化合物,通过选择合适的SPE小柱、优化固相萃取和仪器检测的条件,使该方法在0.050 0 mg/L~1.00 mg/L范围内线性良好。各目标物的方法检出限为0.021μg/L~0.069μg/L,空白水样的加标回收率为36.6%~133%,RSD为0.5%~12.4%。     

气相色谱-三重四极杆质谱法测定水中持久性有机氯污染物

建立了液液萃取一气相色谱三重四极杆质谱多反应监测同时测定水中16种持久性有机氯污染物的方法,考察了不同萃取剂不同体积对有机氯萃取效率的影响,确定了16种持久性有机氯化合物多反应监测模式（MRM）的最佳质谱条件。方法检出限为0.33 ~ 0.65 ng/L,以纯水为基体,加入16种不同浓度水平的持久性有机氯化合物作回收试验,测得回收率在80.2% ~ 103.6%之间,测定的相对标准偏差4.0% ~11.5%（n=7）。     

贵州农作物土壤中OCPs残留现状与差异性分析

通过在贵州主要农作物种植区域采集5 cm、10 cm、15 cm深度的土壤样品,检测其中22种OCPs的残留量。结果表明：在所有水稻土壤样品中除了环氧七氯-A、反式九氯和狄氏剂未检出外,其余19种OCPs均有不同程度检出;OCPs在上述3种深度土壤中总残留量分别为0.526 ng/g、0.497 ng/g、1.605 ng/g。DDTs在3种深度水稻土壤中的总残留量(0.359 ng/g)低于HCHs总残留量(1.135 ng/g)。水稻土壤中γ-HCH、δ-HCH残留量显著高于玉米土壤。水稻土壤中HCHs和硫丹残留主要源自历史上工业制剂的使用,DDTs在水稻土壤中的降解方式主要为厌氧。农作物种植区域土壤中OCPs残留量均符合国家农用地土壤污染风险管控标准。     

无锡某地区土壤中有机氯农药污染状况调查

调查分析了无锡市某地区土壤有机氯农药污染状况。数据表明,该地区土壤有机氯农药主要残留组分为p,p＇-DDE和p,p’-DDT,其浓度处于较低水平,对生态环境和人类健康无显著危害。     

硅胶分离-气相色谱法测定海水样品中的有机氯农药及多氯联苯

建立了硅胶净化-具电子捕获检测器气相色谱(GC-ECD)测定海水样品中有机氯农药(OCPs)、多氯联苯(PCBs)的方法。海水样品经正己烷萃取,浓缩萃取液后过硅胶层析柱,通过梯度淋洗进行样品的净化和分离,采用GC-ECD进行分析测试。OCPs回收率达70.7%~109.2%,PCBs回收率达92.6%~119.2%。采用GC-MS进行辅助确证,结果表明,方法可行。     

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.     

加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中有机氯农药方法研究

通过对加速溶剂萃取、平行蒸发及净化方法等环节的优化实验,建立了加速溶剂萃取-凝胶净化色谱-气相色谱质谱法测定农用地土壤中23种有机氯农药的检测方法。结果表明,方法检出限为0.0034~0.0052 mg/kg;对化合物质量分数为0.25 mg/kg的土壤加标样品进行平行实验,回收率为82.0%~93.7%;测定结果的相对标准偏差（RSD）≤8.7%。对土壤有证标准质控样品进行分析,测定结果均在验收范围之内。该方法准确可靠,灵敏度较高,样品净化效果较好,能够满足农用地土壤中有机氯农药残留痕量分析的要求。