加速溶剂提取-气相色谱法测定蔬菜中的有机氯农药

加速溶剂提取技术萃取蔬菜样品中的有机氯农药残留具有萃取速度快、溶剂用量少、选择性高等优点。用加速溶剂提取-气相色谱法测定蔬菜中的有机氯农药残留,其结果与国标法(GB/T5009,19-1996)和美国EPA法(3545)进行比较。结果表明:加速溶剂提取-气相色谱法能够对蔬菜中多种有机氯农药残留的提取和测定达到很好的效果,蔬菜中12种有机氯农药在两种质量分数(25和100ng·g-1)的添加的回收率在80%和125%之间,高于国标法,而与美国EPA的方法相当。用此法对南京市郊蔬菜中有机氯农药残留状况进行分析表明:南京市郊蔬菜中有机氯农药的检出率在76%和100%之间,DDTs是蔬菜中的主要有机氯农药残留,其次为六六六,分别占残留总量的48.5%~74.6%和14.0%~27.9%。10种试验蔬菜体内DDT和六六六的残留量均不超标,但此类物质可在食物链中富集和放大,仍会对农产品质量和人体健康构成潜在威胁。     

北京官厅水库中有机氯类农药的分布和来源

采用气相色谱/电子捕获检测器法(GC/ECD)对官厅水库表层水体中18种有机氯农药进行分析.结果表明:官厅水库9个采样点水样中18种有机氯农药残留水平为10.06～87.37 ng·L-1,其中∑HCHs和∑DDTs分别为3.93～38.94和3.71～16.03 ng·L-1.官厅水库及其支流水体受到有机氯农药轻度污染,上游工业区废水排放以及各支流周边地区农田排水是官厅水库中有机氯农药的重要来源.与国内外其他地区相比较,官厅水库表层水体中有机氯农药含量较低,∑DDTs、γ-HCH和七氯环氧均未超过GB 3838-2002地表水环境质量标准限值.     

水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法

本研究建立了水体和底泥中8种有机氯农药和5种除草剂的气相色谱-串联质谱(GC-MS/MS)同步测定分析方法.水样以甲醇作为基体改进剂,利用官能化聚苯乙烯/二乙烯苯(PEP)固相萃取柱富集和净化;底泥样品加乙腈用超声波辅助提取,二氯甲烷反萃取,使用氟罗里硅土固相萃取柱净化.采用DB-5MS(30 m×0.25 mm×0.25μm)色谱柱对待测物进行分离,多反应监测模式(MRM)测定.方法的线性相关性均大于0.999.空白水样在低、中、高等3个加标水平下的平均回收率为71%—115%,相对标准偏差(RSD)为4.0%—12.6%,检出限(LOD)0.12—2.0 ng·L~(-1).底泥样品在低、中、高等3个加标水平下,平均回收率为73%—120%,RSD为4.1%—11.0%,检出限(LOD)0.011—0.20μg·kg~(-1).该方法选择性好、灵敏度高且准确可靠,适合于水体和底泥中常见有机氯农药和除草剂类农药的检测.应用该方法测定了东北地区养殖池塘及松花江的水体和底泥样品.结果表明,莠去津检出率最高(100%),水体中残留量在11.2—1671 ng·L~(-1)之间,底泥中残留量在0.35—21.8μg·kg~(-1)之间.有机氯β-六六六检出率80%,水体中残留量在ND—6.76 ng·L~(-1)之间,底泥中残留量在ND—4.74μg·kg~(-1)之间.底泥样品中滴滴涕农药的残留量未超过我国淡水养殖产地环境限量标准.     

微波辅助萃取-气相色谱法检测裙带菜中的多氯联苯和有机氯农药残留

建立微波辅助萃取-气相色谱法同时检测裙带菜中多氯联苯和有机氯农药残留的方法.裙带菜风干、粉碎后,采用微波辅助萃取仪提取粗提液,经净化、脱酸、脱水、浓缩后,用气相色谱-电子捕获检测器进行分析检测.结果表明,本方法多氯联苯和有机氯农药的检出限分别在0.008—0.044 ng.g-1和0.029—0.273 ng.g-1之间,各组分线性相关系数均大于0.996,加标回收率为72%—131%,相对标准偏差在2%—16%之间(n=3).因此,本方法具有节省时间、减少污染、操作简单便捷等特点,可用于裙带菜等海洋藻类中多氯联苯和有机氯农药残留量的检测.     

贵州百花湖水体中有机氯农药的残留及健康风险评价

为了研究贵州百花湖水体中有机氯农药(OCPs)对人体的潜在健康风险,在百花湖及其周边布设8个采样点分别采集水样,采用液液萃取-毛细管气相色谱法对OCPs的残留状况进行测定.结果显示,水样中11种有机氯的总含量范围为15.5～43.8ng·L-1,其中,BHCs和DDTs含量范围分别为3.2～14.6和1.2～7.8 ng·L-1.采用美国国家环境保护局(EPA)推荐的健康风险评价方法的评价结果表明,百花湖水体中OCPs的致癌风险和非致癌风险均低于国际辐射防护委员会(ICRP)推荐的最大可接受风险水平,表明百花湖水体中11种OCPs对人体健康风险处于较低水平.     

气相色谱测定水中19种有机氯农药

建立了毛细管色谱柱/电子捕获检测器-气相色谱法测定19种有机氯农药的的方法,相关系数R2均在0.999以上,方法检出限为4.4×10-3—1.0×10-2mg·L-1,空白样品的加标回收率为91%—109%,相对标准偏差RSD在2.8%—6.6%.通过对萃取次数和萃取溶剂体积实验条件进行优化,测试结果均满足实验要求.     

叶类蔬菜有机氯农药残留测定过程中的提取和净化

用柱萃取法提取 ,气相色谱 电子捕获检测器 (GC ECD)测定蔬菜中的多种有机氯农药 .比较了不同提取溶剂对蔬菜中有机氯农药的提取效率 .就回收率而言 ,正己烷和丙酮 (V/V ,4∶1 ) >石油醚和丙酮 (V/V ,4∶1 ) >二氯甲烷和丙酮 (V/V ,4∶1 ) >纯正己烷 .用正己烷和丙酮作提取溶剂时 ,1 2种有机氯农药中有 1 0种的回收率在 80 %以上 ,变异系数在 1 %— 1 5 %之间 .不同固相萃取 (SPE)填料对有机氯农药的纯化效率为 :硅胶对目标物质的净化效率要高于硅藻土和氟罗里硅土 ,硅胶做填料时变异系数在 1 5 %以下 .因此 ,本实验认为用正己烷和丙酮 (V/V ,4∶1 )做提取剂、选择硅胶做填料能够对蔬菜中多种有机氯农药有较好的提取和净化效果 ,是一种较理想的蔬菜中有机氯农药的分析方法 .     

植物酶膜萃取-气相色谱分析水体中痕量有机磷农药

建立了植物酶膜萃取 气相色谱分析水体中痕量有机磷农药的方法 .实验表明 ,选用精面粉作为酶源并用纯水萃取所得的植物酶最为合适 .乐果、对硫磷和甲基对硫磷三种有机磷农药的检测限为 0 1 μg·l- 1;多次测定三种农药的加标回收率均达70 %以上 .     

沉积物中多环芳烃和有机氯农药定量分析的质量保证和质量控制

以美国ＥＰＡ为方法为基础,进行了沉积物中多环芳烃和有机氯农药分析的质量保证和质量控制实验,采用回收率指示物控制回收率,用内标法定量。结果表明多环芳烃的指示物回收率为５０．６７－９７．３３％,目标化合物的回收率为５８．６７－９６．３３％,方法检测限为３．３０－９．２６μｇ．ｋｇ＾－１。     

厌氧滤池-膜生物反应器处理垃圾渗滤液不同工艺段中有机氯农药残留的分析

建立了基于HLB固相萃取柱和气相色谱／电子捕获(GC／ECD)分析垃圾渗滤液中有机氯农药的分析方法，对厌氧滤池．膜生物反应器处理垃圾渗滤液不同工艺段水体中有机氯农药的浓度进行了分析．结果表明，应用厌氧滤池．膜生物反应器处理垃圾渗滤液可以有效去除有机氯农药残留，主要去除工艺是厌氧，其中P，P’-DDT厌氧反应的中间体产物是P，P’-DDD，大部分继续转化为其它产物．在所试验的垃圾渗滤液中没有检出DDTs和HCHs以外的其它优先控制有机氯农药．     

Residues of organochlorine pesticides (OCPs) in aquatic environment and risk assessment along Shaying River,China

Organochlorine pesticides (OCPs) are pesticides with global scale ubiquity, persistence and bioaccumulation, which leave long-term residuals in the water body. OCPs’ high toxicity poses significant threats to human health and aquatic biodiversity, making assessment of OCPs’ impact on aquatic ecology and human health urgently necessary. In this research, the presence of 16 OCPs in surface water and groundwater along Shaying River, China, as well as OCPs concentration correlations, was investigated at 24 selected sampling sites. At the same time, the ecological risk and human carcinogenic risk were also analyzed by risk quotient method and USEPA’s Risk Assessment Guidance, respectively. Results showed that the total concentration of OCPs ranged from 21.0 to 61.4 ng L^?1 in groundwater, and 12.3–77.5 ng L^?1 in surface water. Hexachlorocyclohexane (HCHs) and heptachlor were the prominent contaminants in groundwater, which indicated their use in the recent past and confirmed their persistence. The α-HCH/γ-HCH ratios in groundwater confirmed that γ-HCH (lindane) was used as main substitute of technical HCH in the study area. The correlation analysis illustrated that δ-HCH and γ-HCH played a dominant role in HCHs residue. Heptachlor and α-HCH, as well as endosulfan and heptachlor epoxide, had a strongly significant positive correlation, suggesting an associated usage of the two pair OCPs. An extremely high ecological risk for aquatic organism was observed for γ-HCH, heptachlor and dieldrin, while the carcinogenic risks posed by the selected OCPs in surface water and groundwater were all acceptable.     

Organochlorine pesticide in water and bottom sediment from Aiba Reservoir (Southwestern Nigeria)

Levels of organochlorine pesticides (OCPs) in water and sediment from Aiba reservoir (Southwestern Nigeria) have been assessed. The aim of the study was to investigate the pollution status of the reservoir water and the bottom sediment. Analytical measurements were carried out for 20 OCPs using standard literature methods. The results showed higher levels of OCPs in the bottom sediment than the water. Significant positive correlations at p<0.05 level were observed for OCPs compounds in water except γ-BHC and endosulfan III, whereas in sediments α-chlordane, dieldrin, endosulfan II, pp-DDT, endrin ketone and methoxychlor did not show any correlation, and aldrin was negatively correlated with pp-DDD. The mean levels of OCPs in both water and sediments were higher, in most cases, than recommended levels for drinking water. Owing to possible toxicity and bioaccumulation tendency of OCPs by the aquatic habitats, the levels of OCPs detected in water and sediment samples could be a source of future health problems. Environmental monitoring of the reservoir is highly recommended.     

广东西江流域饮用水源中典型持久性有机污染物的含量与来源

从广东省西江流域三个饮用水源地采集三个样品,分别分析其中两类持久性有机污染物—有机氯农药和多环芳烃的含量以及来源,从这两类污染物对水环境污染的角度初步判断饮用水源的安全性。首先采用液液萃取的方法对样品进行前处理,然后分别用GC．ECD和GC—MS测定有机氯农药和多环芳烃的含量。实验发现有机氯农药质量浓度在水相中为1．99ng·L^-1～ 4．76ng·L^-1,在颗粒相中为0．36ng·L^-1～0．68ng·L^-1;多环芳烃质量浓度在水相中为73．40ng·L^-1～865．89ng·L^-1,在颗粒相中为16．76ng·L^-1～19．31ng·L^-1。结果表明,六六六和滴滴涕质量浓度低于国标《生活饮用水水源水质标准》（CJ3020．93）的规定,同时苯并[a]芘也低于世界卫生组织《饮用水水质标准》的规定,而其它物质标准中均无规定。由此说明,就有机氯农药和多环芳烃这两类污染物在水中的含量来说,广东西江领域饮用水源是相对安全的。但是由于这两类污染物都具有很强的生物富集性,因此它们在水环境中的存在和作用也是不容忽视的。     

树皮在大气有机氯农药监测中应用的研究进展

有机氯农药(Organochlorine pesticides,OCPs)曾在全世界被大量使用,即使禁用多年,仍能在各种环境介质中被广泛检出,对生态环境和人体健康存在着潜在的威胁。因此OCPs的环境迁移和归趋一直是该领域的研究热点。树皮是一种天然的被动采样器,能够很好的反映出大气有机物长期的污染程度。本文简要论述了树皮作为被动采样器在大气污染物监测研究中应用的优势,并对OCPs在树皮中的残留浓度、特征及影响其富集的因素进行了探讨,最后特别针对具有手性的OCPs在树皮中的对映体选择性特征进行了评述。     

树皮在大气有机氯农药监测中应用的研究进展

有机氯农药（Organochlorine pesticides, OCPs）曾在全世界被大量使用,即使禁用多年,仍能在各种环境介质中被广泛检出,对生态环境和人体健康存在着潜在的威胁。因此OCPs的环境迁移和归趋一直是该领域的研究热点。树皮是一种天然的被动采样器,能够很好的反映出大气有机物长期的污染程度。本文简要论述了树皮作为被动采样器在大气污染物监测研究中应用的优势,并对OCPs在树皮中的残留浓度、特征及影响其富集的因素进行了探讨,最后特别针对具有手性的OCPs在树皮中的对映体选择性特征进行了评述。     

Organochlorine pesticides in soils around Guanting Reservoir,China

Fifty-six representative samples of topsoil were collected around Guanting Reservoir, which is an important water source for Beijing. Concentrations of the insecticides HCH, DDT, and their metabolites were quantified by use of gas chromatography (GC) with electron capture detection (ECD). Organochlorine pesticides (OCPs) are still present in surface soils in the Guanting area. DDT accounts for about 93% of the total OCP content. Concentrations of α/γ, β/γ, and DDT/DDE are the result not only of historical use, but also of more recent depositions. Statistical analyses, including principal component analysis (PCA) and cluster analysis (CA), revealed associations between concentrations of OCPs and major soil characteristics. Geographical information system (GIS) technology was used to develop maps of the distributions of OCP concentrations. The areas of greatest contamination were primarily in the central part of the study area and were correlated with greater population density, heavier traffic, and more industrial activity.     

Assessment of organochlorine pesticide contamination in waterbirds from an agricultural region,Central China

Twenty-one organochlorine pesticides (OCPs) were measured in the muscle of six predominant waterbird species from Jianghan Plain, Hubei Province, Central China. Among OCPs, DDTs were the most prevalent compounds, with average concentration ranging from 31.1 to 1445 ng/g lipid weight. Little egrets (Egretta garzetta) and Chinese pond herons (Ardeola bacchus) showed significantly higher concentrations of OCPs (p < 0.05) due to their dietary habits and migratory patterns. There were no statistically significant differences (p > 0.05) for most OCPs between sex and age groups. The accumulation profiles of HCHs and DDTs suggested that these OCPs in Jianghan Plain were largely derived from historical usage. Risk assessment indicated that heptachlor could be likely to pose adverse health effects on people consuming ducks in Jianghan Plain.     

Organochlorines in the surface sediments of the Bahiret el Bibane lagoon (Tunisia,Southwestern Mediterranean Sea)

Organochlorines (including organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs)) were analysed in 10 surface sediment samples collected from the Bahiret el Bibane lagoon, which is one of the most productive lagoons and one of the most important active commercial fish traps in the southern Tunisia. The aim was to obtain information concerning the recent deposition of these compounds in this area, together with the levels, the distribution and any potential biological risk. Total concentrations of OCPs and PCBs in the sediments ranged from below the limit of detection (?1 and from 29.5 to 88.2?ng?g^?1?dw, respectively. The spatial distribution of PCBs suggested that the sources of these contaminants are probably located outside the lagoon and are transported by water currents and atmospheric deposition. Compared with some other regions of the world, the Bahiret el Bibane lagoon exhibited low to moderate levels of PCBs and OCPs. According to established sediment quality guidelines, PCBs and Lindane at most of the study sites would be more concerned for the ecotoxicological risk in the Bahiret el Bibane lagoon. The results of this study could provide a useful aid for the sustainable marine management of the region.     

Organochlorine pesticides in surface soils and sediments from obsolete pesticides dumping site near Lahore city,Pakistan: contamination status and their distribution

Surface soil and sediment samples were collected from the surroundings of Lila stream, which passes through the obsolete pesticides dumping area Kalashah Kaku near Lahore city, to evaluate the residual levels of 19 organochlorine pesticides (OCPs), their distribution and potential sources. OCPs followed the order: ∑ DDT>∑ HCH>dicofol>endrin>heptachlor>dieldrin. Ratios of β to γ-HCH highlighted an old source of technical HCH in the study area, whereas the predominance of p, p′-DDT and p, p′-DDE indicated presence of technical DDT in surface soils. Factor analysis based on principal component analysis identified the origin of OCPs from industrial activities in Kalashah Kaku and waste dumping from Ittehad Chemical Industries via open drains into Lila stream. Greater levels of DDTs and HCHs above quality guideline pose potential exposure risk to biological organisms, safety of agricultural products and human health in the surrounding of Lila stream.     

长三角地区池塘养殖水产品体内农药类污染与食用风险评价

为了解池塘养殖水产品体内的农药污染情况,以便为水产品质量评价及保障当地居民的饮食健康提供科学依据,本研究采用气相色谱质谱联用法(GC-MS)对长三角地区13个养殖池塘中5类(蟹类、鳖类、蚌类、虾类、鱼类)水产品体内9种有机磷农药(OPPs)、8种有机氯农药(OCPs)以及4种拟除虫菊酯类农药(SPs)进行了检测,并初步分析了其污染来源。结果表明,水产品体内3类农药均有检出,但残留水平均不高,OPPs残留总量为未检出至299 ng·g-1(dw),三唑磷、伏杀硫磷、喹硫磷和毒死蜱较易在水产品体内蓄积;OCPs残留总量为16~82 ng·g-1(dw),主要污染物为六六六(HCHs),主要来自历史残留;SPs残留总量为44~89 ng·g-1(dw),主要污染物为高效氯氟氰菊酯。水产品体内的农药污染可能与养殖池塘中的沉积物污染密切相关。5类水产品体内3类农药的总风险指数(HI)为0.0020~0.046,远小于1,因此,长三角地区由3类农药造成的健康风险处于安全水平。