全自动固相萃取-GC-MS/MS法测定水中多氯联苯

采用全自动固相萃取-气相色谱/三重四极杆串联质谱法(SPE-GC-MS/MS)分析水中7种指示性多氯联苯,通过优化测定条件,使PCBs在0.100μg/L～100μg/L范围内线性良好,方法检出限为0.07 ng/L～0.1 ng/L,回收率为72.1%～102%,RSD为5.8%～12.9%。将该方法用于实际水样测定,结果城市污水处理厂的出水中PCBs检出率较高,而废旧电容器封存点周边地表水易受到PCBs的污染。     

Development,validation of QuEChERS-based method for simultaneous determination of multiclass pesticide residue in milk,and evaluation of the matrix effect

Extraction and quantification of pesticide residue from the milk matrix at or below the established maximum residue limit (MRL) is a challenging task for both analytical chemists and the regulatory institutions to take corrective actions for the human health and safety. The main aim of the study is to develop a simple rapid and less expensive QuEChERS extraction and cleanup method for simultaneous analysis of 41 multiclass pesticide residue in milk by gas chromatography-electron capture detector (GC-ECD), followed by confirmation of the residues with gas chromatography-mass spectrometer (GC-MS). Effect of sorbent type, temperature, spiking concentration, matrix effect (ME), measurement uncertainty (MU), inter- and intra-assay repeatability, reproducibility of recovery, and trueness of the results were investigated to validate the effectiveness of the method. Limit of determination (LOD) and limit of quantitation (LOQ) for all the analytes ranged within 0.001–0.02 and 0.002–0.05 µg mL^?1, respectively. The % recovery of all the pesticides ranged between 91.38 and 117.56% with relative standard deviation (RSD) below 2.79%. The MU for all the analytes was ≤29% of respective LOQs, and except for few pesticides, the ME was largely negative. The method fulfilled all the SANTE guidelines and thus can be extended for routine analysis of multiclass pesticide residue in milk.     

青鳉鱼的行为特征提取研究

采用生物行为传感器获取青鳉鱼的行为数据时,青鳉鱼个体差异会导致采集到的原始电信号在时空特性下完全不同。重要的行为特征往往被隐藏在原始信号中,传统的信号处理方法无法实时而有效地提取到这些特征。针对这个问题,观察并记录了暴露实验前后青鳉鱼的行为变化,提出了一种可以高效表征行为特征的直方图统计算法。实验结果表明,该方法能够准确对应人眼观测到的暴露实验前后鱼的行为变化趋势,同时也为后续异常行为识别提供一定的支持和参考。     

An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal care products in environmental waters

• A hydrophilic resin (GCHM) was facile synthesis and characterized. • Average absolute recovery of GCHM (75.6%) performs better than Oasis^® HLB. • Detection limits of method (SPE-UPLC-MS/MS) ranged between 0.03 and 0.6 ng/L. • 22 PPCPs were determined in environmental waters ranging from 0.5 to 1590 ng/L. In this study, a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-co-divinylbenzene), characterized, and applied as a solid-phase extraction (SPE) material. Up to 44 pharmaceuticals and personal care products (PPCPs) belonging to 10 classes were recovered in environmental water samples. Different variables affecting extraction, such as adsorbent amount, sample pH, and loading speed, were optimized. Under optimal conditions, the average absolute recovery of 44 PPCPs was 75.6% using GCHM, indicating a better performance than the commercial Oasis^® HLB. SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated, and the method achieved good linearity (r²>0.991, for all analytes). In addition, the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L. The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River, Huaihe River, and Taihu Lake, 1 groundwater sample from Changzhou in Jiangsu Province, 1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province, China. In these samples, 22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.     

固体废物中氰化物的浸出特性研究

采用零顶空提取器,对固体废物中氰化物做浸出试验,浸出液用流动注射法测定,并探讨固体废物中影响氰化物浸出的因素。对浸提时间和浸提次数的试验考察可知,冲刷、溶解、吸附、解吸等多种机制作用于浸出的不同阶段。试验表明,当浸提时间为18 h、浸提次数为2次时能将氰化物基本浸提出来;固体废物经稳固化处理后可明显降低氰化物的浸出量,固体废物本身所含的吸附性组分可不同程度地降低氰化物的浸出量。     

间羟基苯甲醛生产废水的处理

研究了萃取法处理间羟基苯甲醛生产废水的工艺条件，并在此基础上进行了废水的生化处理试验。结果表明：萃余液稀释１５倍后用活性污泥法处理，出水ＣＯＤ能达到排放标准。     

Easy and fast extraction methods to determine organochlorine pesticides in sewage sludge,soil, and water samples based at low temperature

Organochlorine pesticides present in sewage sludge can contaminate soil and water when they are used as either fertilizer or agricultural soil conditioner. In this study, the technique solid–liquid extraction with low temperature purification was optimized and validated for determination of ten organochlorine pesticides in sewage sludge and soil samples. Liquid–liquid extraction with low temperature purification was also validated for the same compounds in water. Analyses were performed by gas chromatography-mass spectrometry operating in the selective ion monitoring mode. After optimization, the methods showed recoveries between 70% and 115% with relative standard deviation lower than 13% for all target analytes in the three matrices. The linearity was demonstrated in the range of 20 to 70 µg L^?1, 0.5 to 60 µg L^?1, and 3 to 13 µg L^?1, for sludge, soil, and acetonitrile, respectively. The limit of quantification ranged between 2 and 40 µg kg^?1, 1 and 6 µg kg^?1, and 0.5 µg L^?1 for sludge, soil, and water, respectively. The methods were used in the study of pesticide lixiviation carried out in a poly vinyl chlorine column filled with soil, which had its surface layer mixed with sludge. The results showed that pesticides are not leached into soil, part of them is adsorbed by the sewage sludge (4–40%), and most pesticides are lost by volatilization.     

地面水力压裂对井下煤层瓦斯抽采影响分析

为了研究高河煤矿地面压裂钻井作业对井下煤层瓦斯抽采效果的影响,以3#煤层E2307工作面为主要考察对象,对水力压裂前后煤层渗透率、抽采瓦斯浓度和纯量进行统计分析。研究结果表明:地面压裂钻井水力压裂后煤层反演渗透率提高了13倍以上;压裂后瓦斯浓度最大增幅为122%,最小增幅为34%,平均增幅为71%,同样,瓦斯纯量也有大幅度的提高。研究认为高河煤矿地面水力压裂作业对其高瓦斯含量、低渗透性煤层具有良好的应用前景,对同类煤矿及煤层提高瓦斯抽采效率,预防井下瓦斯动力灾害具有积极的借鉴意义。     

Taking away David’s sling*: environmental justice and land-use conflict in extractive resource development

Exploring cases of gas and coal extraction in Australia and the U.S.A., this paper considers instances in which legal and political frameworks have been used to prioritise development interests and minimise opportunities for community objection. Two case studies illustrate the role of law and the influence of politics on environmental conflict, conflict resolution, and participation in decision-making associated with resource extraction. A range of barriers to meaningful community participation in land-use decision-making are exposed by combining legal and non-legal concepts of equity and justice with ideologies of democracy and representation. These include asymmetry in information and resources available to parties; instances of misrecognition of weaker participants; and examples of malrecognition, where community attempts to engage democratic rights of public participation were thwarted by the strategic and deliberate actions of both industry and government. This paper illustrates the limits of current legal approaches to addressing land-use conflict and contributes to the developing scholarship of environmental justice as an analytic framework for addressing complex environmental and social justice issues.     

Testing the efficiency of extraction of incurred residues from soil with optimized multi-residue method

The reproducibility of extraction of residues from spiked soil samples and from soils containing incurred residues was tested with ¹⁴C-labeled test compounds of different physical-chemical properties. Nearly 100% of the compounds added to the sample before extraction could be recovered with an average reproducibility relative standard deviation (CV) of 5.4%. The additional steps of the determination process (cleanup, evaporation, etc.) contributed to the major part of the variability of the results (CV = 10–20%). The incurred residues were most efficiently extracted with acetone for 30 min followed by the mixture of acetone/ethyl acetate 1:1 for additional 30 min. However, they could only be recovered at various extent (64–90% of total residues), underlying the importance of testing the efficiency of extraction. The residues were identified and quantified by gas chromatography applying thermionic detector. The performance parameters of the method complied with the international method validation guidelines, and they proved to be robust and suitable for determination of pesticide residues in soils of widely different physical–chemical properties.