Determination and health risk assessment of enrofloxacin,flumequine and sulfamethoxazole in imported Pangasius catfish products in Thailand

The goals of this study were to determine the levels of three antibiotics – enrofloxacin, flumequine and sulfamethoxazole – in Pangasius catfish products imported into Thailand and to assess the health risks from consumption. To extract these antibiotic residues, acetonitrile, methanol and a small amount of formic acid were used as solvents. Determination of the antibiotics after extraction steps was carried out by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) technique. The results showed that 14 and 3 samples of Pangasius catfish products were contaminated with enrofloxacin and sulfamethoxazole, respectively. No flumequine residue was found. While the concentration levels of these antibiotics in most contaminated samples were lower than the European Union (EU) standard, one sample was found to contain sulfamethoxazole at 245.91 µg kg^?1, which was higher than the EU standard (100 µg kg^?1), indicating the likelihood that some contaminated freshwater fish products are widely distributed in Thai markets. Notably, the concentration levels of enrofloxacin in samples of Pangasius catfish with skin were higher than in non-skin products, suggesting that products with skin might retain more antibiotic residues than non-skin products. Although the hazard quotient showed that consuming imported Pangasius catfish products, based on the current consumption rate, will not adversely affect consumer health, antibiotic residues in Pangasius catfish products imported into Thailand should be continually monitored.     

Resistance in bacteria and indirect beta-lactamase detection in E. coli isolated from Culex pipiens detected by matrix-assisted laser desorption ionization time of flight mass spectrometry

The aim of this study was detections of antibiotic resistance and resistance mechanism in bacteria isolated from mosquitos (Culex pipiens) living near humans. Therefore, antibiotic resistance in bacteria isolated from Culex pipiens was investigated by disk diffusion test and MIC E-test in this study. MALDI-TOF mass spectrometry was used for detection of resistant mechanism. In this study, hydrolytic breakdown products after a few hours of incubation of the bacteria isolated from Culex pipiens were detected. Results show that enzymatic destruction of ampicillin by beta-lactamases is able to be detected by MALDI-TOF mass spectrometry from wild strains of potential pathogens. The MALDI-TOF mass spectrometry is useful method for routine detection of beta-lactamases resistant mechanism, but overnight incubation of pure culture is necessary. The results are important for proper and fast intervention to limit the spread of beta-lactamase-producing wild bacteria and provide information for appropriate initial therapy of the infections caused by these microbes.     

Seed pre-soaking with 24-epibrassinolide reduces the imidacloprid pesticide residues in green pods of Brassica juncea L.

The effect of 24-epibrassinolide seed soaking on imidacloprid residues in green pods and mature seeds of Brassica juncea L. plants was investigated. The activities of the antioxidative enzymes glutathione-S-transferase, glutathione peroxidase, glutathione reductase, ascorbate peroxidase and guaiacol peroxidase, and the content of glutathione were determined. Imidacloprid residues in green pods were analyzed and quantified by gas chromatography-mass spectrometry, revealing that 24-epibrassinolide treatment resulted in a decrease of residues by almost 30%. In mature seeds, no pesticide residues were detected. Activities of all the antioxidative enzymes and glutathione content were found to be high in plants grown in soil amended with 300 mg imidacloprid kg^?1 soil, but pre-soaking with 100 nmol L^?1 24-epibrassinolide further enhanced the activities of all these enzymes and the glutathione content.     

A Study of Sorptive Loss Patterns for Reduced Sulfur Compounds in the Use of the Bag Sampling Method

In this work, the basic properties of the bag sampling method were examined and characterized in terms of recovery rate with respect to four reduced sulfur compounds (RSC) including H₂S, CH₃SH, DMS, and DMDS. For this comparative study, two types of calibration approaches were performed to evaluate the relative RSC loss due to bag sampling. As a reference calibration tool, a syringe dilution (SD) method was applied. The working standards prepared by diluting the primary standard in a gas-tight syringe (as a mixing chamber) were injected to the GC/PFPD through a loop-injection system to yield a background calibration information. In contrast, the target calibration was performed based on a bag dilution (BD) method. To this end, working standards for multiple calibration points were prepared by two different bag types (Tedlar bag (TB) and polyester bag (PB)). These standards were then drawn by the same syringe and injected into the GC/PFPD via loop. On the basis of these comparative analyses, both absolute and relative differences in RSC recovery rates (RR) were evaluated (e.g., comparison of wall-loss effect). The results indicate that TB has a mean RR of 87% for the four RSC with their values ranging from 82 (CH₃SH) to 91% (DMDS). On the other hand, the results of PB generally exhibited slightly reduced RR with their mean values of 77% (range: 73% of H₂S to 83% of DMS). The results of this study generally suggest that the losses of RSC samples, while inevitable with the bag sampling method, exhibit certain patterns between different RSCs and between different grab sampling materials.     

Short-term Distributions of Reduced Sulfur Compounds in the Ambient Air Surrounding a Large Landfill Facility

In order to explore the environmental behavior of reduced sulfur compounds (RSC) as malodorous components emitted from diverse source processes, the distribution characteristics of four sulfur (S) compounds - hydrogen sulfide (H₂S), methyl mercaptan (CH₃SH), dimethyl sulfide (DMS: (CH₃)₂S), and dimethyl disulfide (DMDS: (CH₃)₂S₂) – were investigated in a municipal landfill area. In the course of this study, their ambient concentration levels were measured during two time periods from 13 individual spots selected as a function of distance from the center of the landfill site. The results generally indicated the absolute dominance of H₂S over the other S compounds investigated (up to 5 km radius) such that their mean values were found as 1415 (H₂S), 148 (DMS), 20.6 (CH₃SH), and 14.4 ppt (DMDS). When our data were compared in terms of either varying distance from the source or relationship with meteorological conditions, the H₂S data sets were most evident to reflect the potential effects of strong source processes in the landfill environment, relative to other S gases (or to volatile organic compounds measured concurrently). The results of this study further indicated the relatively good correspondence between the measured H₂S concentration level and humans' intuitive sensory of odor and nuisance.     

水中酞酸酯类化合物的测定

通过筛选水中酞酸酯类化合物的萃取条件,优选出方法简单、回收率高的萃取方法,利用GC—FID和GC—MS—SIM检测,证明筛选的方法稳定可靠,平均回收率在98．1％～105％,在能力验证中获得了满意的结果。     

固相萃取-GC/MS法测定水中16种有机氯农药

采用HLB固相萃取柱富集水样,乙酸乙酯溶剂洗脱,加入氘代菲作为内标,利用气相色谱/质谱联用法选择离子模式测定水中16种有机氯农药,优化了固相萃取条件。16种有机氯农药在5.00μg/L~250μg/L范围内线性良好,按1 L水样计算,方法最低检出限为1.4 ng/L~19.4 ng/L,相对标准偏差为3.5%~20.0%,平均加标回收率为44.7%~119%。     

南通市开发区化工企业水环境污染源指纹图谱的构建与应用

以南通市开发区化工集中区为应用实施地,不同化工厂不同时间的污染物为研究对象,在GC-MS分析的基础下,联合GIS系统,建立指纹图谱数据库,探索以指纹图谱-GIS联用技术来锁定污染源的方法。结果表明,通过GC-MS初步分析和指纹特征峰的匹配,可快速缩小污染排查范围,为环境监督或污染事故的排查提供一定的技术支持。     

固相微萃取-气相色谱法测定水中甲拌磷及其代谢产物残留

采用固相微萃取技术富集水样中甲拌磷及其代谢产物残留,并用气相色谱法测定。通过优化试验条件,使该方法在0.05 mg/L~1.00 mg/L范围内线性良好,甲拌磷、甲拌磷亚砜和甲拌磷砜方法检出限分别为0.64μg/L、36.1μg/L、1.8μg/L。用该方法测定无公害种植基地的灌溉水样品,3种农药残留均为未检出,水样的加标回收率为60.4%~85.7%,测定5次结果的RSD为3.4%~8.5%。     

水体中磺胺、四环素、喹诺酮类抗生素检测方法

建立了固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)同时检测水体中3类15种抗生素的分析方法。水样用Oasis HLB固相萃取小柱净化富集。通过对比水样在不同pH条件下的回收率,优化了环境水样中抗生素固相萃取过程中的前处理条件。采用甲醇和0.1%甲酸溶液作为流动相,经过梯度洗脱进行分离,在HPLC-MS/MS多反应监测模式下进行定性定量分析。结果表明,环境水体中15种抗生素的检出限和定量下限分别为0.12~1.6 ng/L和0.2~3.0 ng/L,自来水加标回收率为34.9%~102.5%(pH=4)。用该方法对海河流域13个地表水水样进行了初步检测,结果表明,部分抗生素普遍存在于地表水体中。其中,磺胺甲基异NFDA1唑检出频率最高,在13个地表水样品中均有检出。