水中痕量有机磷农药的高效液相色谱/质谱分析

农药对饮用水以及饮用水源的污染在西方发达国家是一项极为关注的课题。有机磷农药作为农药中的一大类,至今仍是世界上生产和使用最多的农药品种。因此,饮用水以及饮用水源中痕量有机磷农药残留的状况受到人们关注。水中痕量有机磷农药的分析方法正在不断地改进,针对ＧＣ／ＭＳ测定某些有机磷农药时存在热分解以及在气相色谱柱上发生吸附的不足。结合高灵敏度、高选择性的质谱鉴定器,本文主要介绍最新的ＨＰＬＣ／ＡＰＩＭＳ方法在水中痕量有机磷农药测定方面的进展和应用。     

部分城市污泥中氯苯类化合物的初步研究

应用GC/MS对我国 1 1个城市污泥中的 5种氯苯化合物 (CBs)进行了研究 .结果表明 ,各城市污泥中CBs的总含量 (ΣCBs)在 0 0 1 0— 6 91 7mg·kg- 1之间 ,绝大部分低于 1 0mg·kg- 1,依次是兰州 >北京 >香港大埔 >无锡 >香港元朗 >广州 >佛山>香港沙田 >西安 >珠海 >深圳 .各城市污泥的CBs都是以个别或少数化合物为主 ,显示出不同的分布特征 ,主要是 1 2 4 三氯苯和六氯苯 ,其它化合物含量普遍较低 .各种CBs化合物的最高含量主要分布于兰州污泥和无锡污泥中 .城市污泥中CBs的含量与污水来源、污水处理方式、污泥类型和CBs化合物的理化性质有关 .     

气相色谱-质谱法测定水稻、土壤及稻田水中的恶庚草烷残留量

建立了一种用于测定糙米、稻壳、植珠（稻草和秧苗）、土壤及稻田水中恶庚草烷残留量的分析方法,样品中的恶庚草烷用乙腈或炳酮提取和微型柱固相萃取净化后,用ＧＣ／ＭＳ（ＳＩＭ）方法测定。仪器的灵敏度低于５０ｐｇ,样品中恶庚草烷的最低检出质量浓度为０．００５ｍｇ／ｋｇ,不同浓度下恶庚草烷的平均回收率为８０．０％－９６．４％,变异系数〈１３％,在恶庚草烷／水稻的残留试验中应用本方法测定恶 草烷残留量取得了满意     

粉煤灰井下填充时PAHs对地下水环境的影响

模拟平煤集团矸石电厂以及焦煤集团演马电厂粉煤灰井下填充过程,设计了静态浸泡和动态淋溶实验,并以固相萃取-气相色谱/质谱联用方法,测定了溶出液中的16种多环芳烃含量.实验结果表明:溶出液中主要的PAHs物质是萘、苊、芴、菲、蒽,均为4环以下的多环芳烃类物质,其含量较低,其中菲和蒽的总含量较高,说明在粉煤灰井下填充过程中,多环芳烃类污染物能够从粉煤灰中迁移至水体,并对地下水环境造成一定的影响.     

Determination of flame-retardant hexabromocyclododecane diastereomers in textiles

To establish a concise and rapid procedure to analyze hexabromocyclododecane (HBCD) diastereomers in flame-retarded textiles, three different methods of extraction—Soxhlet, ultrasonic, and soaking extractions with toluene and dichloromethane (DCM)—were compared. During Soxhlet extraction using toluene, the percent contribution of α-HBCD to total HBCDs increased slightly and that of γ-HBCD decreased, indicating that γ-HBCD was isomerized to some extent at the boiling point of toluene (110.6 °C). For ultrasonic extraction, the temperature of the water bath can easily increase over time during the procedure, which might lead to undesirable effects. Therefore, we considered soaking extraction with DCM to be the most facile procedure to analyze HBCD diastereomers in textiles. Using the method established in this study, commercially available textiles in Japan (n = 10) were analyzed to understand the actual composition of HBCD contents and its diastereomer profiles. With the exception of one textile sample, HBCDs were detected in all the samples analyzed, with concentrations ranging from 22 000 to 43 000 mg kg⁻¹ (i.e. 2.2–4.3%). We found a higher proportion of the α-diastereomer in most textile products compared with that of commercial HBCD mixtures, indicating that γ-HBCD isomerized to α-diastereomer by heating processes to incorporate the commercial formulation into treated materials or that the α-diastereomer preferentially absorbed onto textile materials during the manufacturing of flame-retarded consumer products.     

Persistence of C-labeled atrazine and its residues in a field lysimeter soil after 22 years

Twenty-two years after the last application of ring-¹⁴C-labeled atrazine at customary rate (1.7 kg ha⁻¹) on an agriculturally used outdoor lysimeter, atrazine is still detectable by means of accelerated solvent extraction and LC-MS/MS analysis. Extractions of the 0-10 cm soil layer yielded 60% of the residual ¹⁴C-activity. The extracts contained atrazine (1.0 μg kg⁻¹) and 2-hydroxy-atrazine (42.5 μg kg⁻¹). Extractions of the material of the lowest layer 55-60 cm consisting of fine gravel yielded 93% of residual ¹⁴C-activity, of which 3.4 μg kg⁻¹ was detected as atrazine and 17.7 μg kg⁻¹ was 2-hydroxy-atrazine. The detection of atrazine in the lowest layer was of almost four times higher mass than in the upper soil layer. These findings highlight the fact that atrazine is unexpectedly persistent in soil. The overall persistence of atrazine in the environment might represent a potential risk for successive groundwater contamination by leaching even after 22 years of environmental exposure.     

Risk assessment for human consumption of perfluorinated compound-contaminated freshwater and marine fish from Hong Kong and Xiamen

Perfluorinated compounds (PFCs) are man-made fluoro-surfactants that are identified as global pollutants and can pose health risks to humans and wildlife. Two aspects of risk assessment were conducted in this study, including exposure and response. Exposure was estimated by using the concentrations of PFCs in fish and applying standard exposure factors. Among different PFCs, PFOS, PFOA, PFNA, PFDA, PFUdA and PFTrDA were detected. Total concentrations of PFC in fish ranged from 0.27-8.4 ng g⁻¹ to 0.37-8.7 ng g⁻¹ respectively in Hong Kong and Xiamen. The calculated hazard ratio (HR) of PFOS for all fish was less than 1.0. However, the HR for mandarin fish in Hong Kong and bighead carp, grass carp and tilapia in Xiamen, had HR values of approximately 0.5, indicating that frequent consumption of these 4 more contaminated fish species might pose an unacceptable risk to human health. Our data support the notion that the released/disposed chemical pollutants into water systems make fish a source of environmental toxicants to humans. The risks and potential effects of PFCs to health of coastal population in the Pearl River Delta are of concern.     

超声波萃取-GC/MS法测定橡胶轮胎中的多环芳烃

建立了超声波萃取-气相色谱/质谱(GC/MS)联用测定轮胎制品中多环芳(PAHs)的分析方法.优化了超声波萃取条件,采用MS的选择离子检测方式对PAHs进行定性定量分析.结果表明,16种PAHs的平均加标回收率为75.4%～88.0%,相对标准偏差(n=5)为0.66%～11.90%,方法检出限在1.0～4.0 ng/mL.     

Neurotoxicity and oxidative stress induced by permethrin in gills of the freshwater mussel Unio ravoisieri

Pyrethroids are contaminants found in the aquatic environment, and their toxicological effects on aquatic organisms have received extensive attention. However, the impact on freshwater bivalve of exposure to these chemicals is still largely unknown. Freshwater mussels Unio ravoisieri were exposed to two nominal permethrin (PM) concentrations C1?=?50?µg/L and C2?=?100?µg/L during 7 days. The measured concentrations of PM using gas chromatography (GC/ECD) in the treated aquariums were, respectively, 28.7–62.3?µg/L. Catalase (CAT), Glutathione-S-transferase (GST), and Acetylcholinesterase (AChE) activities, Glutatione (GSH) and Malondialdehyde (MDA) levels were determined in gills of U. ravoisieri. Significant increase in CAT activity by the lowest concentration and decrease by highest concentration were observed. Additionally, GST activity was increased in a concentration-dependent manner. However, statistically significant decrease in GSH levels (about 39%) was observed only at high concentration of this compound (100?µg/L). PM generated an increase in MDA levels reaching the highest value at the high concentration. AChE activity of mussel ranging from 51% inhibition at lowest concentration 50?µg/L to 89% inhibition at highest concentration 100?µg/L. The results indicated that oxidative stress and cell damage might be one of the main mechanisms of PM toxicity to freshwater mussels.