Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

漆酶的逆胶束萃取条件优化的研究

研究了生物表面活性剂逆胶束体系萃取纯化漆酶的后萃的过程.在此逆胶束体系中,表面活性剂采用一种阴离子生物表面活性剂鼠李糖脂(rhamnolipid, RL),溶剂采用异辛烷.分别考察了4种不同离子种类(NaCl, NaBr, KCl和KBr)与不同浓度、4种不同助溶剂种类(正丁醇,正己醇,正庚醇及正辛醇)与不同比例、乙醇的含量以及温度对漆酶的后萃过程的影响.结果表明,0.25mol/L KCl或0.20mol/L KBr能够得到较好的萃取效果;在四种助溶剂中,正己醇(比例为0.5)和正庚醇(比例为0.5)效果比较好;乙醇加入量为9%效果最优;最适宜温度为35℃.在上述条件下,漆酶的酶活回收率和纯化倍数分别高达90%,4.7倍.电泳分析结果进一步证实了漆酶的纯化效果较好.研究证明鼠李糖脂逆胶束萃取酶类具有广阔的应用前景.     

Determination of 4-tert-octylphenol in surface water samples of Jinan in China by solid phase extraction coupled with GC-MS

Octylphenols, considered as xenoestrogens, mainly exist as 4-tert-octylphenol (OP) in aquatic environments. The high stability and accumulation of OP in aquatic systems have caused endocrine disruption. The OP in surface water in Jinan, China was analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with solid phase extraction (SPE). Water samples were extracted by SPE on a cartridge system containing C-18 as sorbent. To increase sensitivity and selectivity, OP was derivatized to 4-tert-octyl-phenoxy silane. With the use of phenanthrene-d10 as internal standard, the detection limit based on signal-to-noise ratio (S/N = 3) was 0.06 ng/mL. The average recovery was from 84.67% to 109.7%. The precision of the method given as the relative standard deviations (RSD) was within the range 6.24%-12.96%. In the target water samples, the concentrations of OP were as follows: 15.88-71.24 ng/L for Jinxiuchuan Reservoir, 3.850-26.68 ng/L for the city moat, 6.930-41.56 ng/L for Daming Lake, 66.03-474.2 ng/L for Xiaoqing River, 14.66-17.72 ng/L for the Yellow River, and 10.60-26.43 ng/L for Queshan Reservoir. The Xiaoqing River was seriously polluted due to the discharge of wastewater from Jinan. Jinxiuchuan Reservoir had a higher concentration of OP compared with the Yellow River and Queshan Reservoir, which is ascribed to the surrounding human activities. These data are reported for the first time, providing strong support for the control of OP pollution in Jinan.     

预富集技术在原子吸收光谱环境分析中的应用

原子吸收光谱法是分析环境水样中金属离子含量的有效方法之一。在测定时往往需要对样品进行前处理,然后再进行测定。文章介绍了近些年较新的一些分离富集技术在原子吸收光谱分析环境中金属离子时的应用,分析了离子交换树脂在样品中金属离子富集分离过程中的研究近况,评述了固相萃取、析相微萃取、单滴液滴微萃取、分散液液微萃取、离子液体萃取、浊点萃取等多种萃取方式在样品预富集中的应用进展,综述了活性炭、纳米粒子、淀粉、分子筛等吸附剂在富集环境水样中金属元素的应用现状,同时还对在线富集技术与流动注射分析技术联用在金属元素分析中的应用进展进行了评述。     

套种条件下混合螯合剂对污染土壤Cd淋滤行为的影响

为了研究螯合剂对污染土壤Cd向下迁移的影响,对采自广东省乐昌市和清远市的2种铅锌矿废水污染水稻土（分别为中性和酸性土壤）进行100 cm土柱室外淋溶试验,研究在玉米与东南景天套种系统中,在5 mmol.kg-1土的混合螯合剂[MC∶柠檬酸∶味精废液∶EDTA∶KCl（摩尔比）=10∶1∶2∶3]的强化作用下对2种污染土壤中Cd的淋滤行为的影响.结果表明,施加混合螯合剂后第2 d,混合螯合剂能明显提高2种土壤各土层淋滤液Cd浓度;施后第8 d混合螯合剂仍能继续提高中性土壤20 cm以下土层和酸性土壤60 cm以下土层淋滤液Cd的浓度,但其活化作用均已迅速下降.施后第2 d和第8 d,2种土壤各土层的套种＋MC处理的淋滤液Cd浓度均超过国家地下水质量标准（GB/T 14848-93）.施加混合螯合剂可降低中性土壤表层全Cd量.不同处理的土壤Cd均有向下层迁移的趋势,尤其是酸性土壤,在20 cm和40 cm处不同处理的全Cd量与起始值比较分别下降了40%～58%和39%～49%,经过100 d的修复即可达到土壤环境质量标准（GB 15618-1995）.上述结果表明,施用混合螯合剂对Cd污染土壤的地下水水质存在一定的潜在污染风险.     

DNA提取方法对活性污泥微生物多样性PCR-DGGE检测的影响

评价超声波法、2种基于SDS的裂解法、改进的化学裂解法、微波法和冻融 玻璃珠 溶菌酶 SDS等6种DNA提取方法对活性污泥微生物多样性PCR-DGGE检测的影响.结果表明,2种不同的DNA纯化方式(溶液和胶纯化)及PCR扩增方式(直接和巢式PCR)对DGGE结果没有明显的影响,但不同的DNA提取方法对DGGE结果有明显的影响,其中2种基于SDS裂解法的DGGE条带较多,其提取的DNA产量(14.85μg/g湿重)和纯度(OD260:OD280＞1.80)也最高;改进的化学裂解法和微波法次之;超声波法、冻融 玻璃珠 溶菌酶 SDS法较少.研究表明,DNA提取方法是影响活性污泥微生物多样性PCR-DGGE检测结果的关键因素,基于SDS的裂解法是用于活性污泥微生物多样性PCR-DGGE研究的一种简便、可靠的总DNA提取方法.     

基于卫星遥感与地面监测分析北京大气NO_2污染特征

分析了1999—2010年北京大气NO2地面质量浓度、2004年以来北京及周边NO2柱浓度的变化.结果表明：1999—2007年来北京大气NO2质量浓度以升高为主.2008年实施奥运空气质量保障措施极大地缓解了北京NO2污染状况,地面质量浓度与垂直柱浓度都出现不同程度的回落.2009年北京大气NO2污染又有所反弹,但低...     

TiO2 nanotubes as solid-phase extraction adsorbent for the determination of polycyclic aromatic hydrocarbons in environmental water samples

An analytical method based on TiO2 nanotubes solid-phase extraction (SPE) combined with gas chromatography (GC) was established for the analysis of seven polycyclic aromatic hydrocarbons (PAHs): acenaphtylene, acenaphthene, anthracene, fluorene, phenanthrene, fluoranthene and pyrene. Factors a ecting the extraction e ciency including the eluent type and its volume, adsorbent amount, sample volume, sample pH and sample flow rate were optimized. The characteristic data of analytical performance were determined to investigate the sensitivity and precision of the method. Under the optimized extraction conditions, the method showed good linearity in the range of 0.01–0.8 g/mL, repeatability of the extraction (RSD were between 6.7% and 13.5%, n = 5) and satisfactory detection limits (0.017–0.059 ng/mL). The developed method was successfully applied to the analysis of surface water (tap, river and dam) samples. The recoveries of PAHs spiked in environmental water samples ranged from 90% to 100%. All the results indicated the potential application of titanate nanotubes as solid-phase extraction adsorbents to pre-treat water samples.     

湘中锑矿区土壤重金属锑的污染特征

文章研究调查了冷水江锡矿山锑矿区、桃江板溪锑矿区、桃江马迹塘锑矿区、桃江武潭锑矿区、安化符竹溪金锑矿区及安化渣滓溪锑矿区及周围土壤中锑的含量及形态分布.结果表明:各矿区土壤中总锑含量范嗣为185.6-2 081.3 mg/kg,大大超过了土壤中锑的背景值,表明各矿区土壤已被严重污染.采用Tessier逐级提取法对土壤中...     

废弃线路板热解油中酚类物质的提取与分离

将FR-4型废弃线路板热解,并对热解油中含量最多的组分-酚类物质进行分离提取.比较研究线路板热解油的分离提取方法,探索出"碱液处理-酸化-萃取-减压蒸馏"的新方法,对分离出的组分进行GCMS(气质联用)测试.结果显示运用该方法对FR-4型线路板的热解油进行提取分离,得到的总酚占热解油的62.0%,其中苯酚的最高纯度可达...