微波萃取技术在分析土壤中有机污染物的应用

介绍了微波萃取技术及其使用的试剂、设备和条件,对微波萃取在分析土壤中有机污染物的应用予以综述,阐述了微波萃取技术是分析土壤中有机污染物的好方法。     

萃取技术在环境样品预处理中的应用及发展

对萃取技术包括传统技术以及新近发展起来的如固相萃取、固相微萃取、膜萃取、超临界流体萃取、微波萃取等技术在环境样品预处理方面的运用进行综述,分析各自的优缺点以及发展前景.     

微波辅助萃取-HPLC-AFS联用技术检测土壤样品中砷的化学形态

建立了微波辅助萃取-高效液相色谱(HPLC)-原子荧光光谱(AFS)联用技术分析土壤中亚砷酸盐[As(Ⅲ)]、二甲基砷(DMA)、一甲基砷(MMA)和砷酸盐[As(Ⅴ)]等4种形态砷。用正交实验设计优化了功率、萃取溶剂体积、萃取温度、萃取时间等微波萃取条件。方法的线性范围为1.00~100μg/L,As(Ⅲ)、DMA、MMA和As(Ⅴ)的检出限分别为0.21、0.33、0.38、0.56μg/L,相对标准偏差为4.6%~5.5%,样品回收率为78.1%~94.4%。用该法分析了4种土壤样品中的砷形态。     

公园地表土中多环芳烃的分离提取及含量分析

比较加压液体萃取法、超声波辅助萃取技术和微波辅助提取技术对公园地表土中多环芳烃的提取效率,并对目标化学成分进行分析鉴定。以超高效液相色谱-三重四极杆质谱作为分析方法,共分离检测出16种多环芳烃类化合物,分别为萘、苊、苊烯、氟、菲、蒽、荧蒽、芘、苯并[a]蒽、艹屈、苯并[b]荧蒽、苯并[k]荧蒽、苯并[a]芘、二苯并[a,h]蒽、茚并[1,2,3-cd]芘和苯并[ghi]苝。结果表明:加压液体萃取法、超声波辅助萃取技术和微波辅助提取技术均可以有效提取公园地表土中多环芳烃类成分。超高效液相色谱-质谱联用技术可以有效地分析公园地表土中多环芳烃类成分。     

微波萃取-双ECD气相色谱法测定土壤中的多氯联苯

建立了利用微波萃取和双ECD联用技术,对土壤中多氯联苯(PCB)的分析方法,通过对回收率、重现性及精密度的测定,其结果均优于传统索氏萃取方法。利用微波萃取可快速、准确、有效地测定土壤中PCB。     

微波-亚临界水萃取底泥中两种多氯联苯的研究

微波亚临界水萃取模拟土样中的2,3-二氯联苯和3,3′-二氯联苯,用气相色谱进行分析。与亚临界水萃取方法相比,该法缩短了萃取时间,分析物的萃取回收率有所提高。对微波亚临界水的萃取条件进行优化,确定了最佳萃取条件为时间20min、温度区段为210℃～225℃。方法对长江镇江段内江的底泥中的多氯联苯进行分析,测定结果与索氏提取-GC分析结果吻合,且不受底泥中腐殖质等有机物影响。     

微波辅助溶样技术及其在环境监测中的应用

微波辅助制样技术是一种快速、低空白、二次污染少、节约能源并降低分析人员劳动强度的样品处理方法。对该技术的原理、特点和操作方法做了简要介绍，并对近年来该技术在生物、空气和废水、土壤和沉积物、固体废弃物等环境样品制备中的应用做了较详细的介绍和评述。     

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.     

痕量有机氯化合物分析中的样品预处理方法

近些年来，痕量有机氯化合物分析中，各种样品预处理技术得到了迅速发展，文章介绍了一些样品预处理方法的原理和最新进展，阐述了索氏提取，超临界流体萃取，微波萃取，固相萃取等几种富集方法的原理，特点，性能及应用，论述了吸附柱层析法，凝胶渗透色谱，高效液相色谱等样品净化技术的特点和应用。     

微波消化-固相萃取光度法测定生物样品中铜的研究

根据试剂2-(4-安替比林偶氮)-5-二甲氨基苯氨(ADA)与铜的显色反应及Waters Plus-C1s固相萃取小柱对显色络合物的固相萃取,结合微波消化样品技术,建立了一种测定生物样品中铜含量的新方法.在pH=4.5 HAc-NaAc缓冲介质中,吐温-80存在下,ADA与铜反应生成2:1稳定的红色络合物,该络合物可用Waters Plus-C18固相萃取小柱富集,富集完后小柱上富集的络合物可用乙醇(含1%HAc)洗脱,洗脱液中铜含量在0-1.0 mg/L内符合比耳定律,摩尔吸光系数ε=5.04×104L·mol-1·cm-1.用微波消化样品后,生物样品中铜含量可用该方法测定.     

微波提取高效液相色谱法测定土壤中15种痕量多环芳烃

采用微波提取结合高效液相色谱技术测定了土壤中15种PAHs的含量.比较了用微波提取、索氏提取和超声萃取3种土壤样品的前处理方法对多环芳烃测定的影响,考察了色谱柱的性能、梯度洗脱条件的优化、荧光检潮波长程序变换及柱温等因素对15种PAHs组分之同分离的影响.经优化后的HPLC方法对15种PAHs的最低检测限为0.10～0.80 μg/kg,相对标准偏差为0.60%～4.60%,方法的回收率为58.1%～97.8%.实验结果表明,该方法兵有高效、快速、灵敏等特点,可以用于环境土壤样品中痕量PAHs的检测.     

Development and application of microwave assisted extraction (MAE) for the extraction of five polycyclic aromatic hydrocarbons in sediment samples in Johannesburg area, South Africa

A microwave-assisted extraction (MAE) method was verified and applied for the extraction of polycyclic aromatic hydrocarbons (PAHs) in sediment samples. Soxhlet extraction was used as the reference method. The optimum MAE was carried out with 20 mL of hexane/acetone (1:1, v/v) mixture in a 1-g sample at 250 W for 20 min. Soxhlet extraction was carried out with 250 mL of dichloromethane:hexane (1:1, v/v) mixture in a 15-g sample for 24 h in a water bath maintained at 60 °C. The collected extracts were both cleaned up, reduced to 1 mL under nitrogen and then injected into an HPLC fluorescence. To increase the sample throughput, simultaneous MAE was performed. The obtained percentage recoveries ranged from 61 to 93 and 88–98 for MAE and SE, respectively. The optimised MAE method was validated using certified reference material. It was then applied to real sediment samples from in and around the greater Johannesburg area. The sediments from Jukskei River were found to be the most polluted while Hartbeespoort Dam sediments were found to be least polluted. The overall order of concentrations for the studied PAHs per site was as follows: Jukskei River?>?Kempton Park?>?Centurion Dams?>?Natalspruit River (PIT)?>?Hartbeespoort Dam.     

Quantification of triazine herbicides in soil by microwave-assisted extraction and high-performance liquid chromatography

A method for the determination of herbicides residues, triazine (atrazine, metribuzin, ametryn, and terbutryn), in soil samples with high-performance liquid chromatography (HPLC)?CUV detection is described. The proposed method is based on microwave-assisted extraction (MAE) of soil samples for 4 min at 80% of 850-W magnetron outputs in the presence of mixture of solvents (methanol/acetonitrile/ethylacetate). Related important factors influencing the MAE efficiency, such as the solvent type and volume, irradiation energy, and time, were optimized in detail. Calibration curve ranges established using HPLC for metribuzin, atrazine, ametryn, and terbutryn are 1.0?C19.0, 0.9?C18.0, 0.6?C11.0, and 0.7?C11.0 µg mL^???1, respectively. The limits of detection of metribuzin, atrazine, ametryn, and terbutryn are 0.30, 0.24, 0.16, and 0.20 µg mL^???1 while limits of quantification are 1.0, 0.80, 0.50, and 0.60 µg mL^???1, respectively. A Plackett?CBurman factorial design was used as a screening method in order to select the variables that influence MAE extraction. The recoveries of the method at three different spiked levels were assessed by analyzing real soil samples and were found to be in the range of 83.33 ± 0.12?C96.33 ± 0.23 with good precision (<8%).     

Determination of organophosphorus fire retardants and plasticizers in wastewater samples using MAE-SPME with GC-ICPMS and GC-TOFMS detection

Determination of organophosphorus fire retardants and plasticizers at trace levels in wastewater is described. In this work, microwave assisted extraction (MAE) and solid-phase microextraction (SPME) are used for sample preparation to extract and preconcentrate the analytes, followed by analysis by gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) for phosphorus-specific detection. Gas chromatography coupled to time of flight mass spectrometry (GC-TOF-MS) was used to confirm the organphosphorus fire retardants in wastewater. The detection limits of organophosphorus fire retardants (OPFRs) were 29 ng L(-1) for tri-n-butyl phosphate (TnBP), 45 ng for L(-1) for tris(2-butoxyethyl)phosphate (TBEP), and 50 ng L(-1) for tris(2-ethylhexyl)phosphate (TEHP). Optimized extraction conditions were performed at 65 degrees C for 30 min and with 10% NaCl. Application of MAE during the sample preparation prior to the SPME allowed the detection of tris(2-ethylhexyl) phosphate, which has been difficult to determine in previous work. Application of the method to wastewater samples resulted in detecting 3.1 microg L(-1) P from TnBP, 5.0 microg L(-1) P from TBEP, and 4.0 microg L(-1) P from TEHP. The presence of these compounds were also confirmed by SPME-GC-TOF-MS.     

基于LSTM-GCN的PM2.5浓度预测模型

应用机器学习算法开展空气质量预测已成为当前研究热点之一,空气质量监测数据具有显著的时空特征,即具有时间维度时序特征和空间维度传输演化特征。面向空气质量监测数据,联合LSTM提取的时间特征和GCN提取的空间特征,提出预测PM_2.5浓度的LSTM-GCN组合模型。以北京市35个空气质量监测站2018—2020年监测数据进行仿真实验,并将LSTM-GCN模型与LSTM模型、GCN模型以及时空地理加权回归模型(GTWR)进行对比,结果显示:LSTM-GCN模型相较于LSTM模型均方根误差(RMSE)、平均绝对误差(MAE)分别降低了11.68%、7.34%;相较于GCN模型RMSE、MAE分别降低了40.22%、36.37%;相较于GTWR模型RMSE、MAE分别降低了17.52%、23.69%,表明所提出LSTM-GCN模型在准确率上有所提升。用LSTM-GCN模型预测2021年1—7月PM_2.5浓度,结果显示预测效果较好。     

Challenges in the application of conventional PCB quantitation methods to studies of "invasive" freshwater organisms

We describe significant and unexpected errors in application of a conventional method for the quantitative determination of polychlorinated biphenyls (PCBs) in unusual biological tissue samples. A standard method based upon microwave-assisted extraction (MAE) and gas chromatography tandem mass spectrometry (GC-MS/MS) was applied to a variety of "invasive" freshwater organisms, representing a variety of genera. The 12 "co-planar" PCBs (co-PCBs) were determined at ng g(-1) levels in small samples (ca. 750-1000 mg) of eight freshwater species (n = 172). We found that the conventional method could lead to random and relatively large changes in retention times. A nearly five-fold increase in retention variability was observed for "lower" organisms compared to that observed in the analysis of predatory fish tissue. These unexpected retention time changes would result in misidentifications, and become problematic not only for non-selective detectors such as electron capture but also for MS-based approaches. That is, for electron impact (EI) ionization methods, molecular ions (M(+)) are produced by loss of Cl not only for congeners in the same homolog class but also for fragments of higher homologs (e.g. M - 35 and M - 37), thereby yielding false positive measurement of the target congener when the retention time windows overlap.     

Spatial Modeling of Mean Annual Temperature in Iran: Comparing Cokriging and Geographically Weighted Regression

Mapping spatial distribution of climatological parameters with a good degree of accuracy is crucial in environmental modeling and planning. Nowadays, there are various models to estimate and predict spatial variables in an area but some such as cokriging and geographically weighted regression (GWR) have got more attention from experts in this field. The objectives of this study are to evaluate and compare GWR with ordinary cokriging (OCK) techniques for estimating the mean annual air temperature (MAT) of Iran using European Centre for Medium-Range Weather Forecasts (ECMWF) data and auxiliary variables (e.g., longitude, latitude and altitude). The MAT-gridded data for Iran was collected in pixels during the time interval of 1987–2015 from the ERA-Interim re-analysis version of ECMWF. Validation results indicate that cokriging model with latitude and altitude for estimating MAT has the lowest MAE (0.0155), MBE (0.00085), RMSE (0.0251), and the highest NS (0.9999) in relation to other cokriging methods. On the other hand, GWR with altitude has better results than those of GWR with other auxiliary variables because of its MAE (0.1271), MBE (0.0124), RMSE (0.1760), and NS (0.9969). By comparing two mentioned methods, cokriging with latitude and altitude has provided the best performance in relation to GWR for prediction of MAT in Iran. To obtain accurate estimation of the spatial distribution of MAT, local residuals were analyzed. Results concluded that residuals of the OCK model have high spatial adaptations between the observed and predicted MAT data compared to the GWR model. Hence, OCK was a relatively optimum method for the estimation of MAT compared with GWR.

     

大气颗粒物中铅污染来源解析技术

近年来,我国大气颗粒物中铅的污染比较严重,其来源比较复杂.大气颗粒物中铅污染来源的解析比较成熟的主要有同位素丰度比、无机多元素分析、质子微探针技术等方法,而序列提取、化学形态分析等技术还处于探索阶段.     

Comparison of DNA extraction methodologies used for assessing fungal diversity via ITS sequencing

Traditional methods of assessing fungal exposure have been confounded by a number of limiting variables. The recent utilization of molecular methods such as internal transcribed spacer (ITS) sequencing of ribosomal RNA genes has provided improved insight into the diversity of fungal bioaerosols in indoor, outdoor and occupational environments. However, ITS analyses may also be confounded by a number of methodological limitations. In this study, we have optimized this technology for use in occupational or environmental studies. Three commonly used DNA extraction methodologies (UltraClean Soil kit, High Pure PCR Template kit, and EluQuik/DNeasy kit) were compared in terms of sensitivity and susceptibility to PCR inhibitors in dust for three common fungal bioaerosols, Aspergillus versicolor, Rhizopus microsporus and Wallemia sebi. Environmental dust samples were then studied using each extraction methodology and results were compared to viable culture data. The extraction methods differed in terms of their ability to efficiently extract DNA from particular species of fungi (e.g. Aspergillus versicolor). In addition, the ability to remove PCR inhibitors from dust samples was most effective using the soil DNA extraction kit. The species composition varied greatly between ITS clone libraries generated with the different DNA extraction kits. However, compared to viable culture data, ITS clone libraries included additional fungal species that are incapable of growth on solid culture medium. Collectively, our data indicated that DNA extraction methodologies used in ITS sequencing studies of occupational or environmental dust samples can greatly influence the fungal species that are detected.