臭氧预氧化处理葡萄酒废水

葡萄酒废水的季节性波动常造成生化处理系统不稳定,使传统的生化处理工艺难以满足新的污水排放标准的要求。研究了臭氧预处理工艺对葡萄酒废水的处理效果及主要控制参数,结果表明,单独的臭氧预氧化对COD几乎无去除效果,但对色度的去除可达到90%;采用O3/H2O2组合工艺可使COD的去除率提高4倍。经臭氧预处理的出水再采用SBR进行好氧处理时,出水COD能降至80 mg/L以下,COD的降解速度及程度都高于未经臭氧处理的稀释原水。高效液相色谱(HPLC)分析显示,经臭氧处理后,除麦芽糖成分被完全去除外,其他各种成分的数量变化不大;GC/MS对废水中多酚类有机物的分析显示,臭氧预处理可将大量难降解的多酚类有机物分解,从而有助于后续生化处理的出水达到更高的污水排放标准。     

植物-微生物联合修复石油污染土壤的实验研究

筛选高效石油降解菌并考察菌株的石油降解能力,通过植物-微生物联合修复石油污染土壤室内实验,在修复过程中测定了土壤中细菌和固氮菌,碱解氮、速效磷和速效钾的含量变化,同时采用傅立叶变换离子回旋共振质谱(ESI FT-ICR MS)考察了植物-微生物联合修复效果。结果表明,菌株3#、4#的生长适应性较强,其混合菌的降解效果最好,将其混合菌液与植物进行植物-微生物联合修复不同浓度的石油污染土壤,经过150 d的温室降解,最高降解率达到73.47%。ESI FT-ICR MS分析结果表明,与空白组相比,植物组的O1、O2和N1类等化合物相对丰度都发生了显著变化,石油污染物得到一定程度的生物降解。     

Analysis of di-n-butyl phthalate and other organic pollutants in Chongqing women undergoing parturition

In this study, 40 healthy women from Chongqing undergoing parturition were recruited and samples of venous blood, umbilical cord blood, breast milk and urine were collected for analysis of organic pollutants by GC/MS. A total of 292 different organic pollutants were detected, including 156 in venous blood, 139 in umbilical cord blood, 176 in breast milk and 138 in urine. Nine different PAEs were detectable in the samples: di-n-butyl phthalate (DBP), bis(2-methylpropyl) phthalate, butyl-8-methyl-nonyl phthalate, di-ethyl phthalate, butyl-2-methylpropyl phthalate, butyloctyl phthalate, di-dodecyl phthalate, di-isodecyl phthalate, and di-tridecyl phthalate. DBP was one of the chemicals detected at the highest frequency (48.82%). DBP concentrations were 84.75 ± 33.52, 52.23 ± 32.50, 57.78 ± 35.42 and 24.93 ± 18.67 μg/l in venous blood, umbilical cord blood, breast milk and urine, respectively. This study represents the first investigation of organic pollutants in a Chongqing population.     

Molecular indicators for pollution source identification in marine and terrestrial water of the industrial area of Kavala city, North Greece

Eight terrestrial and four marine water samples were collected from the industrial section of the city of Kavala in northern Greece to determine the occurrence and distribution of organic contaminants, as well as to identify the molecular markers of different emission sources. The samples were analyzed by means of non-target screening analyses. The analytical procedure included a sequential extraction of the samples, GC-FID, GC/MS analyses, and additional quantitative analyses of selected pollutants. The results show a wide variety of compounds including halogenated compounds, technical additives and metabolites, phosphates, phthalates, benzothiazoles, etc. A close relationship between many of the contaminants and their emission sources was determined based on their molecular structures and information on technical applications.     

On-Site Gas Chromatography/Mass Spectrometry (GC/MS) Analysis to Streamline Vapor Intrusion Investigations

Distinguishing between vapor intrusion and indoor sources of volatile organic compounds (VOCs) is a significant challenge in conventional vapor intrusion assessments. For this research project, the authors developed a step-by-step protocol to streamline building-specific investigations by using on-site gas chromatography/mass spectrometry (GC/MS) analysis and building pressure manipulation to determine the source of VOCs in indoor air during a 1-day field investigation. Protocol validation included implementation in industrial buildings and testing alongside conventional methods. The new protocol compares favorably to conventional approaches, yielding more definitive results in less time. This article presents three case studies which illustrate application of the protocol.     

Distribution of pesticides and bisphenol A in sediments collected from rivers adjacent to coral reefs

To investigate the deteriorating health of coral reefs in Okinawa, Japan, natural sediment samples were analyzed for diuron, Irgarol 1051, chlorpyrifos, and bisphenol A (BPA) which are hazardous to corals. Samples were analyzed by solid-phase extraction (SPE) followed by high-performance liquid chromatography with tandem mass spectrometry (LC–MS–MS). Although diuron and chlorpyrifos usage is only well recorded for farms and not for cities, these chemicals were detected in both rural and urban areas. Additionally, diuron concentration in urban areas was in some cases higher than in rural areas, which might be caused by greater consumption of these chemicals in home gardens in city areas. Irgarol 1051 was detected in downstream river areas, which are situated far from the source sites such as pier or fishery harbor (0.6–3.2 km). This result suggested that Irgarol 1051 could be transported from the river mouths to the sampling sites during flood tides. High BPA concentrations were associated with urban areas (<1.2–22.0 μg kg⁻¹), while low concentrations were associated with rural areas (nd–6.8 μg kg⁻¹). The river sediments under study are delivered to coral reefs in large quantity through runoff caused by typhoons and other heavy rains. The highly hazardous chemicals are carried into coral reefs on these sediments. Therefore, these hazardous chemical substances may already be influencing the coral reefs.     

Formation of multiple trimethylsilyl derivatives in the derivatization of 17α-ethinylestradiol with BSTFA or MSTFA followed by gas chromatography-mass spectrometry determination

N,O-bis(trimethylsily)trifluoroacetamide (BSTFA) and N-methyl-N(trimethylsily) trifluoroacetamide (MSTFA) are common derivatization reagents used in the GC-MS analysis of estrogen steroids such as estrone (E1) and 17(-ethinylestradiol (EE2). In this study, three trimethylsilyl (TMS) steroid derivatives, mono-and di-trimethylsilyl EE2 and mono-trimethylsilyl E1, were observed during the derivatization of EE2 with BSTFA or MSTFA and/or GC separation. Factors influencing the production of multiple TMS derivatives and their relative abundance were examined. It was found that both methanol and bisphenol A competed with estrogenic esteroids when reacting with silylation reagents, and thus affected the formation of TMS derivatives and their relative abundance in the derivatization products. Methanol was found to be more reactive than bisphenol A with the BSTFA reagent. None of the three solvents tested in this study could prevent the generation of multiple TMS derivatives during the derivatization of EE2 with BSTFA, followed by GC analysis. A similar result was observed using MSTFA as the derivative reagent followed by GC analysis. Thus, the suitability of BSTFA or MSTFA as the derivatization reagent for the determination of E1 and EE2 by GC-MS, under the conditions reported here, is questionable. This problem can be solved by adding trimethylsilylimidaz (TMSI) in the BSTFA reagent as recommended, and the performance of the method has been proved in this study.     

空气预浓缩气相色谱/质谱法测定南京环境空气中二硫化碳

采用不锈钢采样罐采集全量空气样品,使用空气预浓缩冷冻的方法从空气样品中提取二硫化碳,经气相色谱/质谱仪测定,判断确定空气恶臭物质的种类和污染来源。方法的最低检测浓度为0.003mg/m3,能够满足中国(TJ36-79)居住区大气中有害物质二硫化碳的最高容许浓度0.04mg/m3(一次值)标准的测定要求。     

改进的QuEChERS-LC/MS/MS法快速检测蔬菜中7种农药残留

研究建立了蔬菜中农药多残留的快速检测QuEChERS-LC/MS/MS方法,优化了实验方案,样品以0.1%乙酸的乙腈（V/V）作为溶剂,Agilent Bond Elut提取试剂盒对样品进行1 min提取后,用C18和Agilent Bond Elut净化试剂盒净化。结果表明：7种农药的平均回收率为72%～127%,相对标准偏差为1.3%～16.3%,检出限为0.004～0.022 mg·kg^-1。该方法减少了溶剂用量,缩短了检测时间,每个样品溶剂用量仅为20 mL,每个样品的前处理费用大约为30元,一个实验人员每日可以处理50～60个蔬菜样品,真正实现农残的快速、简便、廉价、有效、灵敏、安全检测。     

苯醚甲环唑在番茄和土壤中的残留动态研究

采用田间试验方法研究苯醚甲环唑在番茄和土壤中的残留与降解动态,应用超高效液相色谱-串联四级杆液质联用法(UPLC-MS/MS)进行定性和定量分析. 结果表明,苯醚甲环唑在番茄中的平均回收率为90.3%～107.1%,变异系数为0.7%～7.8%;在土壤中的平均回收率为80.1%～104.7%,变异系数为7.2%～9.1%. 动态研究结果表明:苯醚甲环唑在番茄中的降解比在土壤中快,在山东和河南两地番茄中的降解半衰期分别为3.3～3.8和3.3 d;在土壤中的降解半衰期分别为19.9～22.4和13.1～18.8 d. 10%苯醚甲环唑微乳剂在番茄上按照推荐剂量最多施药2次,采收期距最后一次施药3 d,番茄中苯醚甲环唑残留量小于0.158 mg/kg. 低于日本和澳大利亚规定的最高残留限量(MRL,0.5 mg/kg),说明苯醚甲环唑为低残留、易降解农药.