Evaluation and validation of two different chromatographic methods (HPLC and LC-MS/MS) for the determination and confirmation of ochratoxin A in pig tissues

This study was undertaken to compare two different analytical methods for the determination and confirmation of ochratoxin A (OTA) in blood serum, kidney and liver of pigs. Sample clean-up was based on liquid-liquid phase extraction. The detection of OTA was accomplished with high-performance liquid chromatography (HPLC) combined either with fluorescence detection (FL) or electro spray ionization (ESI+) tandem mass spectrometry (MS–MS). Comparative method evaluation was based on the investigation of 90 samples of blood serum, kidney and liver per animal originating from different regions of Serbia. The analytical results are discussed in view of the respective method validation data and the corresponding experimental protocols. In general, analytical data obtained with (LC–MS–MS) liquid chromatography electro spray tandem mass spectro metry detection offered comparable good results at the sub-ppb concentration level. The results indicate that the liquid chromatography electro spray tandem mass spectrometric (LC-MS/MS) method was more specific and sensitive for the analysis and confirmation of ochratoxin A in pig tissues then high pressure liquid chromatography (HPLC) method after methylation of OTA.     

能源利用中烃类气体检测技术研究进展

烃类气体作为地表油气地球化学勘查地下油气藏的直接指标,以及钻井液检测中指导钻井作业的重要因素,在挥发性烃类污染控制中也发挥着重要作用。通过对各类烃类气体检测技术现状和应用情况进行分析与整理,为该类技术针对不同目标的选择与组合提供了依据。     

炸药废水中TNR含量直接光度法测定的研究

以三硝基间苯二酚 ( TNR)溶于水后 ,溶液呈现出明显的亮黄色 ,据此直接用光度法对炸药废水中 TNR的含量进行了测定 ,并论证了光度法的测试条件。同时以消解测氮法进行印证 ,结果表明方法具有可行性     

模拟车用工况下5kW燃料电池尾气净化系统

模拟了车用工况下燃料电池发动机脉冲式排氢的特点,设计开发了一套质子交换膜燃料电池的尾气净化系统,并以5 kW燃料电池的尾气排放为例,研究其净化效果。研究了电池阳极排放氢气缓冲前后尾气中氢气浓度的变化,以及不同空速条件下氢气的去除效果。结果表明：电堆阳极排放氢气经过缓冲处理后,尾气中氢气浓度趋于平稳,大部分工况下处在2%以下,达到了安全处理的要求;尾气中氢气的去除效果与空速密切相关。对自制的整体式催化剂而言,当空速低于20000 h^-1时,氢气的去除率能达到约95%,而当空速达到39270 h^-1时,氢气的去除率仅为10.9%。鉴于这一问题,提出通过采用尾排空气的分流手段调整催化燃烧反应器对空速的要求,以提高尾气中氢气的去除率。     

Matrix effect on the performance of headspace solid phase microextraction method for the analysis of target volatile organic compounds (VOCs) in environmental samples

Solid phase microextraction (SPME) is a fast, cheap and solvent free methodology widely used for environmental analysis. A SPME methodology has been optimized for the analysis of VOCs in a range of matrices covering different soils of varying textures, organic matrices from manures and composts from different origins, and biochars. The performance of the technique was compared for the different matrices spiked with a multicomponent VOC mixture, selected to cover different VOC groups of environmental relevance (ketone, terpene, alcohol, aliphatic hydrocarbons and alkylbenzenes). VOC recovery was dependent on the nature itself of the VOC and the matrix characteristics. The SPME analysis of non-polar compounds, such as alkylbenzenes, terpenes and aliphatic hydrocarbons, was markedly affected by the type of matrix as a consequence of the competition for the adsorption sites in the SPME fiber. These non-polar compounds were strongly retained in the biochar surfaces limiting the use of SPME for this type of matrices. However, this adsorption capacity was not evident when biochar had undergone a weathering/aging process through composting. Polar compounds (alcohol and ketone) showed a similar behavior in all matrices, as a consequence of the hydrophilic characteristics, affected by water content in the matrix. SPME showed a good performance for soils and organic matrices especially for non-polar compounds, achieving a limit of detection (LD) and limit of quantification (LQ) of 0.02 and 0.03 ng g⁻¹ for non-polar compounds and poor extraction for more hydrophilic and polar compounds (LD and LQ higher 310 and 490 ng g⁻¹). The characteristics of the matrix, especially pH and organic matter, had a marked impact on SPME, due to the competition of the analytes for active sites in the fiber, but VOC biodegradation should not be discarded in matrices with active microbial biomass.     

Development and application of LC–APCI–MS method for biomonitoring of animal and human exposure to imidacloprid

Imidacloprid (IMI) is a relatively new neuro-active neonicotinoid insecticide and nowadays one of the largest selling insecticides worldwide. In the present study a LC–APCI–MS based method was developed and validated for the quantification of imidacloprid and its main metabolite 6-chloronicotinic acid (6-CINA) in urine and hair specimens. The method was tested in biomonitoring of intentionally exposed animals and subsequently applied for biomonitoring of Cretan urban and rural population.     

苯并噻吩脱硫菌株的筛选及脱硫活性研究

从孤岛油田油浸土样中筛选到1株能降解苯并噻吩(BT)的脱硫菌,经初步鉴定该菌为戈登氏菌属(Gordona sp.).实验证明:该菌能以类似于4S途径脱除BT及其衍生物中的硫,但是不能脱除二苯并噻吩(DBT)及其衍生物中的硫.GC-MS分析表明该途径的终产物为邻羟基苯乙醛或其异构体苯并呋喃.在以BT为唯一硫源的培养基中30℃培养48h,Gordona sp.C-6能降解0.15mmol/L的BT,终产物占发酵培养基中BT加入量的50%,其余BT在有氧培养过程中挥发.通过Matlab拟合曲线确定以邻羟基苯乙酸为标准品进行产物定量检测的方法.     

石油化工企业有限空间中的气体检测

介绍了便携式气体检测报警仪用于石油化工企业中有限空间的气体检测时的采样方法、检测点选择、检测工作程序以及检测结果的处理.     

新型汽车尾气净化催化剂的研究

研究Ｌａ－Ｃｏ－Ｃｕ－Ｍｎ－Ｃｅ－Ｐｄ催化剂的活性和热稳定性,结果表明,该催化剂具有低温活性良好、活性高以及热稳定性好的性能特点,对ＣＯ、ＨＣ氧化的Ｔ５０％和Ｔ１００％分别约为１８２℃,２３８℃和２４０℃、２６５℃,催化剂表面组分发生强相互作用形成３种活性中心,是催化剂低的起燃温度,高活性的原因。催化剂高温处理后未发生烧结,活性未下降,热稳定性良好。