液相色谱串联质谱法同时测定水中26种抗生素

建立了一种高效液相色谱串联质谱法同时测定水中26种痕量水平抗生素的分析方法。采用HLB柱对500 mL pH=2.0水样进行固相萃取,用2%氨水-甲醇/乙腈(1∶1,V/V)洗脱,浓缩定容至1.0 mL。选择C18色谱柱,0.1%甲酸水-甲醇作为流动相对目标物进行分离,采用正离子电离模式测定,内标法定量。结果表明,26种抗生素的检出限为0.4～2.1 ng/L,目标物在0～500μg/L范围内,相关性良好(R>0.994),精密度为3.8%～17%,痕量水平下回收率范围为63.1%～102%。该方法简便、快速、准确、涵盖目标物种类多,适用于水质中抗生素的多残留同时测定。     

南京北郊大气细粒子硝基苯酚类化合物污染特征与来源

硝基苯酚类化合物是大气中普遍存在的一类含氮有机物,也是大气吸光性有机物(即棕色碳)的重要组成部分,对气候变化、空气质量和人体健康都具有重要影响.自2019年3月至2020年1月于南京北郊地区采集了共265个大气细粒子(PM2.5)日样品,并利用超高效液相色谱质谱联用仪(UHPLC-MS)定量分析样品中的8种硝基苯酚类化...     

往复流砾石床水质净化效果研究

研究了往复流砾石床对雨污混合流脱氮效果的影响,试验设计两个相同的砾石床系统,采用回流与间歇流同步的进水方式,通过调控水位和停留时间使砾石床内部循环往复运行复氧,同步实现时间和空间上的硝化反硝化过程,分析在两种水力负荷(132 mm·d-1和158 mm·d-1)条件下干湿交替对污染物的去除效果的影响.结果表明:相同配水...     

Effcient degradation of lube oil by a mixed bacterial consortium

A laboratory study was performed to assess the biodegradation of lube oil in bio-reactor with 304# stainless steel as a biofilm carrier. Among 164 oil degrading bacterial cultures isolated from oil contaminated soil samples, Commaonas acidovorans Px1, Bacillus sp. Px2, Pseudomonas sp. Px3 were selected to prepare a mixed consortium for the study based on the e ciency of lube oil utilization. The percentage of oil degraded by the mixed bacterial consortium decreased slightly from 99% to 97.2% as the concentration of lube oil was increased from 2000 to 10,000 mg/L. The degradation of TDOC (total dissolved organic carbon) showed a similar tendency compared with lube oil removal, which indicated that the intermediates in degradation process hardly accumulated. Selected mixed bacterial consortium showed their edge compared to activated sludge. Scanning electron microscopy (SEM) photos showed that biofilms on stainless steel were robust and with a dimensional framework constructed by EPS (extracellular polymeric substances), which could promote the biodegradation of hydrocarbons. The increase of biofilm followed first-order kinetics with rate of 0.216 g glucose/(cm2 day) in logarithm phase. With analysis of Fourier transform infrared spectroscopy (FT-IR) and gas chromatography-mass spectrometry (GC-MS) combined with removal of lube oil and TDOC, mixed bacterial consortium could degrade benzene and its derivatives, aromatic ring organic matters with a percentage over 97%.     

Enantioselective separation and zebrafish embryo toxicity of insecticide beta-cypermethrin

Enantioselectivity of chiral pollutants is receiving growing concern due to the difference in toxicology and environment fate between enantiomers.In this study,enantiomers of insecticide beta-cypermethrin (beta-CP) were separated on selected chiral column by HPLC,and the toxicity of enantiomers was evaluated using the zebrafish embryo-larval assays.The enantiomers of beta-CP were baseline separated on Chiralcel OD and Chiralpak AD columns and detected by circular dichroism (CD) at 236 nm.Better separation could be achieved at lower temperature (e.g.,20°C) and with lower levels of polar modifiers.Pure enantiomers were obtained on Chiralcel OD.The CD spectra of enantiomers were recorded.By comparing the elution order with a previous similar study,the absolute configuration of beta-CP enantiomers was determined.The individual enantiomers were used in zebrafish embryo test,and the results showed that beta-CP enantioselectively induced yolk sac edema,pericardial edema and crooked body.The 1R-cis-αS and 1R-trans-αS enantiomers showed strong developmental toxicities at concentration of 0.1 mg/L,while the 1S-cis-αR and 1S-trans-αR induced no malformations at higher concentration (e.g.,0.3 mg/L).The results suggest that the enantioselective toxicological effects of beta-CP should be considered when evaluating its ecotoxicological effects.     

海洋环境沉积物中氯霉素残留量的测定

应用高效液相色谱法测定海洋环境沉积物中的氯霉素残留.本方法的线性范围是0.5 ×10-9 ～ 5 ×10-9,其相关系数为0.997,最低检出浓度为0.09 ×10-9,回收率在85.1% ～ 95.8%之间,相对标准偏差小于3.6%.该方法快速、灵敏、定量范围宽,检测结果准确可靠,应用性强.     

在线固相萃取液质联用法测定饮用水源中的痕量联苯胺

建立了在线固相萃取液相色谱串联质谱法测定水中痕量联苯胺的方法。样品经自动进样器注入在线固相萃取小柱后,用富集泵流动相实现对样品的富集洗脱,然后用分析泵流动相将样品从富集柱冲洗至色谱柱后用串联质谱仪进行检测。该方法可在11 min内自动完成对样品的富集、净化、进样和检测过程。当进样量为5 mL时,联苯胺在0.010~2.0 μg·L-1范围内具有良好的线性关系,相关系数R为0.999,检出限为0.8 ng·L-1,实际水样的回收率为85%~104%。该方法具有简单、快速、重现性好、灵敏高等特点,可用于环境水体中痕量联苯胺的检测。     

植物-固体菌剂联合修复石油污染土壤的基础研究

以高效石油降解菌N2、KB为目的菌种,玉米粉、麸皮和锯末为载体制备固体菌剂,并测定了这3种载体的饱和持水量、pH值和吸菌量。以吸菌量为评价指标,结合经济性综合选择最优载体,同时还考察了温度、pH值和料水比对最优载体吸菌量的影响。通过测定微生物数量和石油降解率的变化,考察了植物微生物联合修复效果。结果表明,与玉米粉和麸皮相比,锯末饱和持水量更大、吸菌量较大。锯末是木材厂的下脚料,可以实现高价值资源化利用。在温度30℃,pH为7,料水比1：1.5的最适培养条件下,固体菌剂中N2和KB两种细菌的活菌数量分别高达1.00×109CFU·g-1和1.58×109 CFU·g-1。采用生物菌剂和柳枝稷对石油污染土壤进行植物-微生物联合修复实验,100 d后石油降解率可达到50.5%。     

水体中27种有机磷阻燃剂(OPFRs)的检测及风险评价

有机磷阻燃剂(organophosphorus flame retardants,OPFRs)具有致畸、致癌、致突变风险以及神经毒性作用。为了更好地研究其存在水平和健康风险,建立了固相萃取与高效液相色谱-串联质谱仪和气相色谱-质谱联用仪检测水体中27种OPFRs的分析方法,并对OPFRs进行了健康风险评价。20种OPFRs采用MCX固相萃取柱预处理和LC-MS/MS进行检测,以甲醇和含10 mmol·L⁻¹的甲酸水溶液作为流动相进行梯度洗脱,7种OPFRs采用HLB串联Envi-18固相萃取柱进行预处理并利用GC-MS进行检测。检测结果表明,27种OPFRs的检出限为0.02~2.53 ng·L⁻¹;定量限为0.06~8.43 ng·L⁻¹;回收率为65.82%~108.48%。2021年4月份,采集北京市潮白河地表水和地下水8个水样并检测其OPFRs。实测结果表明：除磷酸三(2-异丙基苯)酯、磷酸异癸基二苯酯、磷酸叔丁基苯二苯酯、磷酸二苄酯外,其余23种OPFRs均有不同程度检出,质量浓度为0~973.17 ng·L⁻¹;磷酸三(2-乙基己基)酯、磷酸三乙酯、磷酸三丙酯、磷酸三异丙酯含量相对较高,分别高达973.17、459.90、315.47、298.41 ng·L⁻¹。采用USEPA模型对水样中的OPFRs进行了健康风险评价, 13种OPFRs的非致癌风险值为0~6.17×10⁻⁴,4种OPFRs致癌风险值为1.37×10⁻⁹~1.07×10⁻⁷;在高暴露条件下,OPFRs的非致癌风险值为1.61×10⁻⁵~6.17×10⁻⁴,致癌风险值为1.00×10⁻⁸~1.07×10⁻⁷,均低于风险阈值。上述结果说明,水体中OPFRs产生的健康风险处于较低水平。此次采集的潮白河地表水和地下水水中OPFRs的致癌风险和非致癌风险均处于较低水平。本研究结果可为地表水和地下水水体中OPFRs的检测及风险评价提供参考。     

用氧化铝厂赤泥制备高效混凝剂聚硅酸铁铝

研究了以氧化铝厂赤泥为原料，在常压通氧条件下，用稀硫酸浸取制备高效混凝剂聚硅酸铁铝（PSAF）的方法，确定了合理的生产工艺和操作条件。该混凝剂用于处理工业废水，并与聚合硫酸铁（PFS）的处理效果比较，CODCr和色度去除率分别提高约20%和28%，SS去除率提高约10%，同时，探讨了该混凝剂处理废水的反应机理。