Speciation of mercury in South African coals

Total mercury (Hg_TOT) concentrations were determined by inductively coupled plasma mass spectrometry (ICP MS) for South African Highveld coals. The distribution of Hg in coals was investigated using a four-stage sequential leaching protocol and isotope dilution/gas chromatography coupled to ICP MS (ID-GC-ICP MS). The results show that Hg_TOT ranged from 144 to 303?µg?kg^?1 with a mean of 199?±?26?µg?kg^?1, while Hg_TOT leached from coals using different solvents ranged between 103 and 310?µg?kg^?1 (mean: 218?±?60?µg?kg^?1). Hg leaching rates of 53–78% were achieved in crushed coals. Hg⁰, Hg²⁺, and CH₃Hg⁺ were identified in all coals. CH₃Hg⁺ in studied coals ranged between 0.1 and 0.4 (mean: 0.2) µg?kg^?1. GC ICP MS chromatograms also showed unknown Hg peaks which were identified as other organomercury species such as ethylmercury. Modes of occurrence of Hg in coals were variable with the organic-bound (37–40%) and the sulfide-bound (37–39%) being the dominant mercury forms. Increasing the HCl concentration in the used protocol increased the amount of Hg leached (16%) during this step.     

The efficacy of an oxidation pond in mineralizing some industrial waste products with special reference to fluorene degradation: a case study

The efficacy of the oxidation pond on the outskirts of the 10th of Ramadan, the main industrial city, in Egypt was examined. Samples of wastewater collected from the inlet and the outlet were screened for some priority pollutants. Acenaphthene and fluorene were the most frequently detected polycyclic aromatic hydrocarbons, while dimethyl phthalate was the most frequently detected phthalate ester. The spectrum of pollutants, their concentrations and frequencies were similar in the inlet and the outlet, indicating an inferior mineralization capability of the pond. Several degradative bacterial strains were isolated from the pond and grown on M56 minimal media supplemented with different pollutants as the carbon source. The efficacy of pure and mixed cultures to break down fluorene, the most frequently detected pollutant was examined. Fluorene degradation was fast in the first 10 days, then followed by a slow phase. Mixed culture had a higher rate of fluorene degradation in comparison to pure cultures. High performance liquid chromatography analysis of fluorene degradation showed three degradative metabolites. But GC/MS analysis detected one compound, identified as acetamide. The present work has indicated the poor efficacy of the pond. Lack of primary treatment of industrial effluent at factory level, coupled with shock loads of toxicants that may damage the microorganisms and their degradative capabilities are presumably main factors behind such inferior performance. Moreover, the type of pollutants discharged into the pond tend to fluctuate and change depending on the rate from the factories discharge and work shifts. Such irregular feeding of persistent pollutants may have led to a wash out of specialized strains of bacteria capable to degrade such persistent pollutants.     

土壤样品多氯联苯的GC/ECD双柱测定方法的优化

GC/ECD法是目前测定土壤样品多氯联苯（PCBs）总量最常用的方法.笔者参考US EPA 8082方法,针对实际土壤样品基质复杂、浓度差别大、有机氯农药干扰GC/ECD测定等特点,对样品前处理和仪器分析的各个环节进行了系统的试验研究.采用碱解萃取、酸洗、硅胶柱净化、双柱GC/ECD分析方法,将多元线性回归分析用于混合Aroclor污染类型的定性识别,外标法用于PCBs总量的定量分析.PCBs总量的清洁基体加标回收率为80%～90%,方法检出限为0.40 ng/g.      

SPE-RRLC-MS/MS法测定制药废水中青霉素G

建立了利用固相萃取-高分离度快速液相色谱-串联质谱(SPE-RRLC-MS/MS)测定制药废水中青霉素G残留的方法。水样以30%硫酸锌+20%亚铁氰化钾作为沉淀剂沉淀蛋白质后,上清液采用Oasis HLB固相萃取柱富集和净化,以0.01 mol/L乙酸铵溶液(加0.1%甲酸)+乙腈作为流动相进行等度洗脱,经Agilent Plus C18柱分离后,在串联质谱ESI(+)源下进行MRM检测。该方法的青霉素G检出限(S/N=3)为0.02μg/L,目标物在0.0020～1.0 mg/L范围内线性关系良好,线性相关系数为0.9997。在0.20,1.0,2.0μg/L添加水平平均回收率为74.6%～101.4%,相对标准偏差为4.49%～8.17%。该方法灵敏度高、重现性好、定性定量准确,可满足制药废水中青霉素G残留检测的要求。     

Comparative in vitro metabolism of chloroxylenol,chlorophene, and triclosan with rat,mouse, and human hepatic microsomes

A number of studies have reported the presence of chlorinated phenols, commonly used as antiseptics, in the environment. Chloroxylenol, chlorophene, and triclosan are three such chemicals believed to have leached into water supplies through the wastewater treatment facilities. Understanding how these compounds are metabolized is important in determining the risks of chemical exposure. In this study, we compared the in vitro metabolism of these three chlorinated phenols with rat, mouse, and human liver microsomes. The structures of the metabolites formed during the microsomal reactions were identical when rat, mouse, and human liver extracts were used, but variations existed in the kinetics of the reactions.     

Determination of pentachlorophenol in human urine using solid phase extraction and GC‐MS analysis with stable isotope dilution

A method for the determination of pentachlorophenol (PCP) in human urine was developed. Urine samples were fortified with ¹³C₆‐IabeIed PCP and hydrolyzed with sulfuric acid prior to extraction. The urine samples were then passed through preconditioned solid phase extraction cartridges containing octadecylsilane adsorbent. The PCP was subsequently eluted from the cartridge with ethyl acetate and converted to pentachloroanisole prior to GC‐MS analysis. GC‐MS quantitation was performed using the technique of stable isotope dilution. Percent recoveries averaging 100, 97, and 111% were obtained for replicate urine samples fortified with approximately 2, 20, and 200 ng/mL of PCP, respectively. The method detection limit was estimated to be 0.2 ng/mL.     

Analysis,accumulation and central effects of trihalomethanes. I. bromoform†

The paper presents the results obtained in a study on the effects of organic micropollutants on the central nervous system of the rat, used herein as a suitable model for neurotoxicologic work. Bromoform, a member of the trihalomethane (THM) family, was the pollutant selected since it becomes a characteristic marker in the Barcelona potable water supply.

Analytical data on the GC‐ECD separation of THMs from other volatile halocarbons is presented. A mixed packed column 10% SE‐30/PEG 20M (94:6) at 70°C provides an adequate separation. The distribution of bromoform in rat plasma and tissues showed an accumulation in brain, kidney and fat, increasing in this order and a rapid elimination after 30 min. The effect on the central aminergic metabolism is studied by HPLC. The increased metabolic activity detected could be attributed either to an increased nervous activity, stimulating the metabolism of serotonin, or to its greater degradation.     

基于液相色谱法分析水环境中大环内酯类抗生素污染的研究进展

大环内酯抗生素广泛使用,在水环境中的残留越来越引起世界关注.本文综述了国内外基于液相色谱技术分析水环境中大环内酯的方法,比较不同预处理法以及分析方法的灵敏度和检出限.固相萃取法可以同时富集和净化,消耗试剂少,方便,野外操作可行,是理想的预处理技术.液相色谱串联质谱技术选择性好、特异性高、灵敏度高,可以检测浓度低于ng.L-1的目标物,是一种可靠理想的分析方法.最后对大环内酯分析研究进行了展望.     

采用代谢流量分析方法评估二噁英对细胞的代谢干扰

以肝癌细胞HepG2为供试细胞,选用5个不同浓度的二噁英（0、0.001、0.01、0.1和1.0 nmol.L-1）,探讨2,3,7,8-TCDD对HepG2细胞的毒性效应.采用90%甲醇离心法实现蛋白与代谢产物的分离,建立了高效液相色谱-串联三重四极杆质谱（HPLC-MS/MS）分析胞外液中的23种代谢产物（20种氨基酸、乳酸、甘油和尿素）的方法.建立的HPLC-MS/MS分析方法对各化合物的加标回收率可达91%—105%之间,化合物浓度的标准偏差均小于10%.在此基础上,结合代谢流量分析系统研究了2,3,7,8-TCDD对HepG2细胞内代谢流的影响.结果表明,随着浓度的增高,2,3,7,8-TCDD对HepG2细胞代谢的干扰作用呈增强趋势.2,3,7,8-TCDD降低了细胞对葡萄糖的吸收,并进一步抑制了HepG2细胞糖酵解的速率.此外,2,3,7,8-TCDD导致了HepG2细胞乳酸代谢流的明显增加,由此使细胞产生了过量的乳酸.     

环境中氟喹诺酮类抗生素残留检测和去除研究进展

环境样品中的氟喹诺酮类抗生素(FQs)残留浓度低,干扰因素复杂,其检测需要采用多个预处理步骤,固相萃取回收率和重现性好,在实际样品预处理中常采用。检测方法包括毛细管电泳分析法、酶联免疫吸附法以及LC与ECD、FLD、UV、MS联用等。毛细管电泳法速度快,敏度低,检出限高;酶联免疫吸附法检测速度快,但存在交叉反应。高效液相色谱联用质谱检测(HPLC-MS/MS)灵敏度高,选择性好,是比较理想的分析方法。FQs污染物降解方法包括污泥吸附、光降解和高级氧化。光降解和高级氧化技术成本较高,反应副产物可能存在环境风险。污泥颗粒吸附FQs效果好,吸附FQs后,污泥颗粒可通过高温碳化活化制备活性炭,使FQs在高温下得到较彻底降解的同时,实现污泥的资源化利用,是较具前景的去除FQs的方法。