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.     

Screening Capsicum chinense fruits for heavy metals bioaccumulation

Elevated concentrations of heavy metals in edible plants could expose consumers to excessive levels of potentially hazardous chemicals. Sixty-three accessions (genotypes) of Capsicum chinense Jacq, collected from 8 countries of origin were grown in a silty-loam soil under field conditions. At maturity, fruits were collected and analyzed for seven heavy metals (Cd, Cr, Ni, Pb, Zn, Cu, and Mo) concentrations. The main objectives of this investigation were: 1) to determine the concentrations of seven heavy metals in the soil and monitor their accumulation in mature fruits, 2) to categorize the pepper accessions as low or high heavy metal accumulators, and 3) to determine if heavy metal content of the pepper fruit was lower than the permitted limits. Concentrations and relative proportions of heavy metals in pepper fruits of C. chinense varied among accessions. Fruits of Plant Introduction (PI) 355820 accumulated significant concentrations of Cd (0.47 μ g g^?1dry fruit). PI-260522 accumulated the highest concentration of Pb (2.12 μ g g^?1 dry fruit) among the 63 accessions tested. This accession (PI-260522) contained about twice the Pb limit on a fresh weight basis. Among the 63 accessions analyzed, PI-238051 contained the highest levels of Ni (17.2 μ g g^?1). We concluded that high accumulator genotypes may be useful for phytoremediation, while, low accumulator accessions might be appropriate selections for growing on Cd-, Pb-, or Ni-contaminated soils to prevent potential human exposure to heavy metals and health hazards through the food chain.     

高气速间歇式生物过滤去除高负荷H2S

采用生物过滤法,以鸡粪堆肥和PE混合物为填料,在高气速条件下间歇式处理高负荷H2S废气。空床停留时间为20、15、10、6.7和5 s时,入口浓度3 000 mg/m3下的平均去除率分别为100%、100%、96.5%、89.2%和90.5%。高气速EBRT为5 s时,高入口负荷2 147 g/(m3.h)时的去除负荷为2 023 g/(m3.h),去除率达94%。采用Michaelis-Ment-en模型进行生物降解宏观动力学研究,其中Ks为550 mg/m3,Vm为6.8×104g/(m3.d)。结果表明,在实验温度17～24℃,湿度30%～50%下,生物过滤法间歇式处理高气速高负荷H2S的去除性能好。     

Plant steroid hormones produced under Ni stress are involved in the regulation of metal uptake and oxidative stress in Brassica juncea L

Brassinosteroids (BRs) are involved in the amelioration of various biotic and abiotic stresses. With an aim to explore the role of BRs under heavy metal stress, plants of Brassica juncea L. were grown in pots. The plants were subjected to various concentrations of Nickel metal (0.0, 0.2, 0.4 and 0.6 mM) and harvested on 60th day in order to observe the expression of these hormones. The isolated BRs from the leaves of Brassica plants characterized by GC-MS include 24-Epibrassinolide (24-EBL), Castasterone, Dolicholide and Typhasterole. The effect of isolated 24-EBL was studied on Ni metal uptake and antioxidative defense system in 60 d old plants of Brassica. It was observed that 24-EBL significantly increased the activities of stress ameliorating enzymes and lowered the metal uptake in plants. This is the first report in B. juncea L. plants showing the expression of BRs under metal treatments and effect of the isolated 24-EBL on metal uptake and in oxidative stress management.     

The structure of the fire fighting foam surfactant Forafac®1157 and its biological and photolytic transformation products

For several decades, perfluorooctane sulfonate (PFOS) has widely been used as a fluorinated surfactant in aqueous film forming foams used as hydrocarbon fuel fire extinguishers. Due to concerns regarding its environmental persistence and toxicological effects, PFOS has recently been replaced by novel fluorinated surfactants such as Forafac®1157, developed by the DuPont company. The major component of Forafac®1157 is a 6:2 fluorotelomer sulfonamide alkylbetaine (6:2 FTAB), and a link between the trade name and the exact chemical structure is presented here to the scientific community for the first time. In the present work, the structure of the 6:2 FTAB was elucidated by ¹H, ¹³C and ¹⁹F nuclear magnetic resonance spectroscopy and high-resolution mass spectrometry. Moreover, its major metabolites from blue mussel (Mytilus edulis) and turbot (Scophthalmus maximus) and its photolytic transformation products were identified. Contrary to what has earlier been observed for PFOS, the 6:2 FTAB was extensively metabolized by blue mussel and turbot exposed to Forafac®1157. The major metabolite was a deacetylated betaine species, from which mono- and di-demethylated metabolites also were formed. Another abundant metabolite was the 6:2 fluorotelomer sulfonamide. In another experiment, Forafac®1157 was subjected to UV-light induced photolysis. The experimental conditions aimed to simulate Arctic conditions and the deacetylated species was again the primary transformation product of 6:2 FTAB. A 6:2 fluorotelomer sulfonamide was also formed along with a non-identified transformation product. The environmental presence of most of the metabolites and transformation products was qualitatively demonstrated by analysis of soil samples taken in close proximity to an airport fire training facility.     

高分子量高纯度阳离子聚丙烯酰胺的合成

以丙烯酰胺与丙烯酰氧乙基三甲基氯化铵为单体,在复合引发剂的作用下,选择水溶液共聚法合成高分子量与高纯度阳离子型聚丙烯酰胺(CPAM)。实验表明,有机偶氮引发剂A用量0.5‰、氧化还原引发剂用量0.45‰、还原剂与氧化剂摩尔比2∶1、反应体系pH为4与反应时间5 h条件下,CPAM分子量为1 042万,且溶解性好。通过对聚合物残单含量影响因素添加剂用量、反应时间的研究,结果表明,添加剂EDTA和增溶剂D对残留AM含量影响小,而苯甲酸钠对聚合物残留AM的含量影响显著;延长反应时间至7 h,残单含量可降低至0.27%,CPAM的纯度高。通过与国内外3种同类型产品进行对比,结果表明,自制产品的分子量明显高于其他产品,且残单含量比国内产品降低了50%～75%。     

高硬度富锶地下水的软化沉淀-超滤膜联用工艺

针对一种高硬度富锶地下水,分别采用石灰和石灰-碳酸钠两种方法,利用药剂软化/超滤膜工艺对其进行软化处理,同时考察了药剂投量对出水锶含量的影响。结果表明,采用石灰软化/超滤膜法,Ca(OH)2最佳投加量为270 mg/L时,出水总硬度(以CaCO3计)由287.12 mg/L降低到96.44 mg/L,硬度去除率为66.41%,出水锶含量也由原水中的0.37 mg/L下降为0.21 mg/L;而采用石灰-碳酸钠软化/超滤膜法,Ca(OH)2和Na2CO3最佳投加量分别为270 mg/L、160mg/L时,出水总硬度降低到60.34 mg/L,硬度去除率达78.98%,锶含量仅为0.02 mg/L。2种处理方法出水总硬度均达到预期目标,石灰软化/超滤膜法可使出水锶含量满足富锶水的要求,而石灰-碳酸钠软化/超滤膜法则造成了对人体有益微量元素锶的大量损失。     

高效聚合氯化铝对超滤膜污染影响的中试研究

针对某水厂以超滤为核心的短流程水处理工艺,在通过聚氯乙烯(PVC)超滤膜之前选择不同投加量(5、10、15和20 mg/L)的高效聚合氯化铝(HPAC)对长江下游原水进行混凝处理。通过跨膜压差(TMP)增长趋势、CODMn的去除率以及混凝后的水质,可知HPAC的最优投加量为15 mg/L。在此投加量下,运用体积排阻色谱法分析原水、膜前水、膜后水中各相对分子质量有机物的变化,可以发现混凝去除有机物的效果要优于超滤截留的。继而将HPAC与另外4种常用混凝剂:硫酸铝(分析纯)、氯化铁(化学纯)、聚合氯化铝(PAC)、聚合硫酸铁进行对比,结果表明,在它们各自最优投加量下,HPAC能够更有效地减缓超滤膜TMP的增长率,从而降低膜污染。因此,认为HPAC是与PVC超滤合金膜契合效果最佳的混凝剂。     

UV/Fenton技术处理某工厂高浓度乳化油废水

研究了UV/Fenton技术对高浓度金属清洗乳化油废水的处理效果,考察了亚铁与双氧水浓度、pH、反应时间和搅拌对COD去除效果的影响。实验结果表明,UV/Fenton技术对高浓度乳化油废水(COD平均浓度为35 000 mg/L)具有较高的去除效果,最佳工艺条件为:亚铁与双氧水浓度分别为2 400 mg/L和6 000 mg/L,pH为3,经过2 h反应,COD可降低至1 050 mg/L,去除率为97%。搅拌会降低COD的去除率。研究表明,UV/Fenton技术对高浓度乳化油废水具有很好的降解效果,且药品消耗较低,为目前此类高浓度有机废水的处理提供了技术参考。     

盐析分相微萃取—高效液相色谱法测定水中含氯除草剂

采用盐析分相微萃取—高效液相色谱法同时测定水中3种含氯除草剂,建立并优化了反相离子对液相色谱条件,考察了萃取剂种类、盐析剂的种类和加入量及试样pH对萃取效果的影响。对氯苯氧乙酸、2,4-二氯苯氧乙酸和2,4-滴丁酯的质量浓度在0.1~100.0mg/L内与色谱峰面积呈良好的线性关系,相关系数不低于0.9992。平均回收率分别为96.29%、79.16%和70.21%,相对标准偏差小于5.3%。该方法操作简便、绿色环保,适合于水中含氯除草剂的测定。