混合表面活性剂-浊点萃取法测定沉积物中多环芳烃的含量

以混合型表面活性剂（十二烷基硫酸钠（SDS）和对叔辛基苯基聚己二醇醚（Triton X-114））为萃取剂,采用浊点萃取法萃取沉积物中的15种多环芳烃（PAHs）,并利用HPLC技术测定15种PAHs的含量。实验结果表明,当混合型表面活性剂的加入量 3％（w）、混合型表面活性剂中SDS含量 50%（φ）、Na2SO4含量 8％（w）、萃取温度 60 ℃、超声萃取时间 10 min 时,15种PAHs的线性关系良好,r=0.998 9~0.999 7,检出限0.4~8.2 μg/L,加标回收率71.22%~97.36%,相对标准偏差0.92%~4.36%（n=6）。     

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil –effect of extraction methods

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45–3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present.     

Trace level determination of selected sulfonylurea herbicides in wetland sediment by liquid chromatography electrospray tandem mass spectrometry

Sulfonylurea herbicides are widely used in crop production on the Canadian prairies and a portion of these herbicides applied to cropland are inevitably lost to surrounding aquatic ecosystems. Little is known regarding the presence of sulfonylurea herbicides in wetlands located amongst cropland. This paper describes a new analytical method for the extraction and the determination of seven sulfonylurea herbicides (thifensulfuron-methyl, tribenuron-methyl, ethametsulfuron-methyl, metsulfuron-methyl, rimsulfuron, nicosulfuron and sulfosulfuron) in wetland sediment. The method provided > 85% analyte recovery from fortified sediment for six of the seven sulfonylurea herbicides with a limit of quantification (LOQ) of 1.0 μ g kg^{? 1}. Tribenuron-methyl had significantly lower recovery compared to the other six sulfonylurea herbicides (LOQ = 2 μ g kg^{? 1}). Mean recovery standard deviations were < 10%. This methodology was used to quantify sulfonylurea herbicide residues in sediment samples collected from prairie wetlands situated within the agricultural landscape of Saskatchewan and Manitoba, Canada. This is the first-known detection of sulfonylurea herbicide residues in prairie wetland sediments. Ethametsulfuron-methyl, sulfosulfuron and metsulfuron-methyl, the three most environmentally persistent of the seven sulfonylurea herbicides monitored in the surveillance component of this study, were most frequently detected in wetland sediment with mean concentrations ranging from 1.2 to 10 μ g kg^{? 1}.     

Simultaneous analysis of thiabendazole,carbendazim and 2-aminobenzimidazole in concentrated fruit juices by liquid chromatography after a single mix-mode solid-phase extraction cleanup

A method using liquid chromatography and a single mix-mode solid-phase extraction cleanup for the simultaneous analysis of thiabendazole [2-(1,3-thiazol-4-yl)-1H-benzoimidazole], carbendazim [(methyl N-(1H-benzoimidazol-2-yl)-carbamate)] and 2-aminobenzimidazole (1H-benzimidazol-2-amine) in concentrated fruit juices is described. The three fungicides were isolated from the samples and concentrated by solid-phase extraction on Oasis MCX cartridges. The determination was performed by liquid chromatography with a diode array, detecting at 288 nm. In this method, the average recoveries from blank control juice samples spiked in a concentration range of 0.01–0.10 mg/kg were in the range of 81–95%, with relative standard deviations below 8%. Detection limits and limits of quantification were 4 μ g/kg and 10 μ g/kg, respectively, for each fungicide. Real juice samples were analyzed by the proposed method. The results were compared to those from liquid chromatography-tandem mass spectrometry.     

Selective separation of deltamethrin by molecularly imprinted polymers using a β-cyclodextrin derivative as the functional monomer

A deltamethrin-imprinted polymer (MIP₁) was prepared using bis(-6-O-butanediacid monoester)-β-cyclodextrin (BBA-β-CD) as the functional monomer and toluene 2,4-diisocyanate (TDI) as the cross-linker. In comparison to the molecularly imprinted polymer where β-CD was applied as the functional monomer (MIP₂), MIP₁ showed a higher specific binding capacity (ΔC_P) and an improved imprinting factor (IF) for deltamethrin. The selective recognition experiments demonstrated that compared to MIP₂, MIP₁ could better recognize its template over other substrates that had similar chemical structures. The solid phase extraction (SPE) of deltamethrin using MIP₁ as the adsorbent was further investigated. The recoveries of the molecularly imprinted solid phase extraction (MISPE) column for deltamethrin were 83.2–93.4% with relative standard deviations (RSD) of 2.03–6.19%. The method has been successfully applied to the enrichment of trace deltamethrin from real water samples.     

Comparison of Microwave Assisted Extraction with Conventional (Homogenization,Vortexing) for the Determination of Incurred Salinomycin in Chicken Eggs and Tissues

Abstract

Incurred and fortified salinomycin residues were extracted from chicken tissues and eggs by homogenization, vortexing and by microwave assisted extraction. The salinomycin residues were quantitated by liquid chromatography following postcolumn derivatization with either vanillin or 4-dimethylamino-benzaldehyde and detected at 520 or 592 nm, respectively. Comparison of residue data indicated that microwave assisted extraction performed as well as the vortexing technique in extracting salinomycin residues in the tissues of laying chickens that were fed meal containing drugs at various level. In the present study, extracts from homogenizing could not be analyzed directly without clean up. Therefore, microwave assisted extraction appears to be a reliable, reproducible, and economical substitute for routinely used homogenization and vortexing extraction techniques.     

酸浸法提取煤矸石中Al2O3的研究

煤矸石是主要的煤系固体废物,其中Al2O3质量分数约占35％左右.以某煤矿的煤矸石为原料,通过单因素实验比较盐酸和硫酸对Al2O3的浸取率,研究各因素对Al2O3浸取率的影响,确定浸取煤矸石中Al2O3的最佳酸浸介质为硫酸.利用正交实验确定酸浸取的最佳条件为:液固比(酸溶液体积与煤矸石样品质量比)15 mL/g、硫酸摩尔浓度3 mol/L、浸取时间120min、助样比(助溶剂与煤矸石样品质量比)0.20,在此条件下硫酸对煤矸石中A12O3的浸取率可达79.6％.     

2种分步浸提方法对土壤中Cr形态提取效果的比较

实验模拟了受铬渣污染的土壤环境,比较在不同活性炭加入量下2种典型分步浸提方法:Tessier 5步法和改进的7步分离方法得到的不同结果,探究适合于铬渣污染对土壤环境的铬形态浸提方法。实验结果表明,2种方法的浸提数据虽有较大差异,但能得到相对一致的变化趋势;七步法形态分类更为细致,99%以上的铬都分布在2~3个结合形态,Tessier五步法的物料衡算结果更为准确(96%~103%),相比七步法形态分类更具包容性,数据更具重现性;随着活性炭的加入,土壤环境中游离铬离子明显减少,转化为有机结合态等更稳定的结合形态,说明活性炭能有效固定土壤环境中游离的铬离子,增加其迁移稳定性。     

Leaching Characteristics of Heavy Metals and As from Two Urban Roadside Soils

The leaching tests, including the Toxicity Characteristic Leaching Procedure (TCLP), EDTA extraction and BCR sequential extractions before and after EDTA treatments, were performed on two specific soils to elucidate heavy metal-associated mineral fractions and general leachability. The TCLP illustrated the low leachability of heavy metals in soils from two sites. EDTA is a strong chelator and therefore had higher extraction efficiency compared to that of TCLP. The lower extraction percentages by EDTA for As and Sb were found compared to the other heavy metals derived from anthropogenic sources. Sequential extractions showed that the importance of acid-extractable, organically-bound and Fe–Mn oxide fractions was identified for anthropogenic heavy metals with the exception of As and Ni while the importance of residual fraction was identified for endogenous metals. Changes in sequential fractions of heavy metals after leaching with EDTA are very complex and it is difficult to generalize on which fraction was more mobile than the others. These combined results are helpful in elucidating the association of heavy metals to soil fractions and the mobility characteristics of heavy metals under certain environmental conditions.     

Environmentally friendly assessment of organic compound bioaccessibility using sub-critical water

The evaluation of microbial availability of contaminants is of high importance for better reflecting the processes governing contaminant fate in soil and for establishing the risk associated with contaminated sites. A sub-critical water extraction technique was assessed for its potential to determine the microbially degradable fraction of [¹⁴C]phenanthrene-associated activity in two dissimilar soils at three different ageing times (14, 28 and 49 days). For the majority of determinations, no significant (p > 0.05) difference between sub-critical water-extracted ¹⁴C-activity at 160 °C and the fraction mineralized by catabolically active Pseudomonas sp. was observed. Collectively, the results suggested that the sub-critical water extraction technique was an appropriate technique for predicting the biodegradable fraction of phenanthrene-associated ¹⁴C-activity in dissimilar soils following increasing soil-contaminant contact time.