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.     

页岩气开采中压裂废液处理技术的发展及应用

作为新型的天然气资源,近年来页岩气的开采力度不断增加。文章广泛调研页岩气开采过程中的场地修复、压裂废液处理等方面的环境污染风险,国内外现行压裂废液的处理工艺,系统分析了中和法、絮凝法和氧化法等处理工艺,并结合实际应用效果和企业需求对技术发展方向进行了预测,可为非常规油气资源开发领域提供理论参考。     

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.     

乳状液膜法处理煤制兰炭废水

以磷酸三丁酯(TBP)为载体、煤油为膜溶剂、NaOH水溶液为内水相,采用乳状液膜法处理兰炭废水。实验结果表明:当TBP体积分数为4%、表面活性剂质量分数为4%、内水相NaOH质量分数为12%、油内比(乳状液的油相与内水相的体积比)为3∶2、乳水比为1∶5、萃取时间为15min时,废水中的酚类(以苯酚计)去除率达到85%以上,COD去除率达83%以上。     

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。     

Kinetics study of fermentative hydrogen production from liquid swine manure supplemented with glucose under controlled pH

Kinetics of H₂ production from liquid swine manure supplemented with glucose by mixed anaerobic cultures was investigated using batch experiments under four different pH conditions (4.4, 5.0, 5.6, and uncontrolled). The temperature for the experiments was controlled at 37 ± 1°C and the length of experiments varied between 50 and 120 hours, depending upon the time needed for completion of each individual experiment. The modified Gompertz model was evaluated for its suitability for describing the H₂ production potential, H₂ production rate, and substrate consumption rate for all the experiments. The results showed that the Gompertz model could adequately fit the experimental results. The effect of pH was significant on all kinetic parameters for H₂ production including yield, production rate and lag time, and the substrate utilization rate. The optimal pH was found to be 5.0, at which a maximum H₂ production rate (0.64 L H₂/h) was obtained, and deviation from the optimal pH could result in substantial reductions in H₂ production rate (0.32 L H₂/h for pH 4.0 and 0.43 L H₂/h for pH 5.6). The results also showed that if pH was not controlled for the batch fermentation process, the substrate utilization efficiency could steeply decrease from 98.8% to 33.7%.     

Parental phenols exposure and spontaneous abortion in Chinese population residing in the middle and lower reaches of the Yangtze River

Widespread use of phenols has led to ubiquitous exposure to phenols. In experimental animals, phenols increased resorptions, reduced live litter size and fetal body weights. However, there are limited epidemiological evidences of the relationships between exposure to phenols and pregnancy outcomes. We evaluated the associations between parental urinary levels of various phenols and spontaneous abortion in a Chinese population residing in the middle and lower reaches of the Yangtze River. A case-control study was conducted that included 70 case couples with medically unexplained spontaneous abortion and 180 control couples who did not have a history of spontaneous abortion and had at least one living child. Both parental urinary phenols were measured by ultra-high performance liquid chromatography-tandem mass spectrometry including bisphenol A (BPA), benzophenone-3 (BP-3), 2,3,4-trichlorophenol (2,3,4-TCP), pentachlorophenol (PCP), 4-n-octylphenol (4-n-OP) and 4-n-nonylphenol (4-n-NP). Compared with the low exposure group, there was an increased risk of spontaneous abortion with high paternal urinary PCP concentration [odds ratio (OR) = 2.09, 95% Confidence Interval (CI), 1.05–4.14], and maternal exposure to 4-n-OP and alkylphenol(s) also significantly increased the risk of spontaneous abortion (OR = 2.21, 95% CI, 1.02–4.80; OR = 2.81, 95% CI, 1.39–5.65, respectively). Our study firstly provides the evidence that paternal PCP exposure, maternal 4-n-OP and alkylphenol(s) exposure are associated with spontaneous abortion in humans.     

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.     

云母钛珠光颜料的应用研究

介绍了一种不使用有机溶剂获得云母钛珠光颜料、水性金属效果云母钛珠光浆、珠光涂料的环保型制备工艺和性能.采用液相沉积法获得了不同厚度的纳米TiO2薄膜包覆层而显示银白、金、红、紫、蓝、绿等各种色彩的系列珠光云母颜料;应用珠光云母颜料与分散剂等水性助剂混合,获得了水性金属效果云母钛珠光浆的制备工艺;应用云母钛珠光浆与乳液配合,获得了云母钛珠光涂料的制备工艺.制备的云母钛珠光涂料系列多彩,白度高、反射率大、珠光效果好,硬度、附着力、耐候性等指标优异.