Determination and occurrence of endocrine disrupting compounds,pharmaceuticals and personal care products in fish (Morone saxatilis)

Endocrine disrupting compounds (EDCs), pharmaceuticals and personal care products (PPCPs) have attracted much attention due to widespread contamination in aquatic environment. In this study, we determined 13 EDCs and PPCPs in fish blood, bile and muscle by using gas chromatography-mass spectrometry (GC-MS). The limits of quantitation (LOQ) were in the ranges of 0.23–2.54, 0.22–2.36 ng·mL⁻¹, and 0.24–2.57 ng·g⁻¹ dry weight (dw) for fish blood, bile and muscle, respectively. Recoveries of target compounds spiked into sample matrices and passed through the entire analytical procedure ranged from 65% to 95%, from 60% to 92% and from 62% to 91% for blood, bile and muscle, respectively. The methods were applied to the analysis of fish from a lake in California. Target compounds were relatively low in bile, and only bisphenol A (BPA) and diclofenac were measurable near the LOQ. Seven of 13 compounds were detected in blood, with total concentrations up to 39 ng·mL⁻¹. Only BPA was frequently found in muscle, with mean concentration of 7.26 ng·g⁻¹ dw. The estimated daily intake of BPA through fish consumption for U.S. resident was significantly lower than the tolerable daily intake recommended by the European Food Safety Authority. This study showed that the exposure to the bisphenol A from fish diet is unlikely to pose a health risk.     

PSE-UPLC-MS/MS法测定污泥中9种药物与个人护理品

利用加压溶剂萃取法(PSE)提取、固相萃取法净化并结合超高效液相色谱-串联四极杆质谱仪(UPLC-MS/MS)检测,建立了污水处理厂污泥中7个药剂类别的9种药物与个人护理品(舒必利、咖啡因、美托洛尔、氯霉素、萘啶酸、卡马西平、驱蚊胺、氯贝酸、苯扎贝特)的分析检测方法.在萃取方法中,对加压溶剂萃取的污泥质量和溶剂进行了优化;在净化方法中,对固相萃取柱种类、固相萃取柱容量、洗脱溶剂和洗脱量进行了优选.结果表明,方法检出限(以干质量计,下同)在2.7～65.0 pg/g范围内,加标回收率在67.0%～130%之间,相对标准偏差均小于25%(即标准偏差小于25 μg/L).应用所建立的分析方法,对北京某污水处理厂的脱水污泥进行了测定,9种目标物质含量为nd(未检出)～50.5 ng/g,其中,舒必利、咖啡因、卡马西平、驱蚊胺和氯贝酸在2010年春、夏季2次采样均有检出.      

Biodegradation of trace pharmaceutical substances in wastewater by a membrane bioreactor

The biodegradation of selected pharmaceutical micropollutants, including two pharmaceuticals with argued biodegradation, was studied by a lab-scale membrane bioreactor. The reaction kinetics and affecting factors were also investigated in this paper. Clofibric acid (CA) with contradictive biodegradation reported was degraded almost completely at different hydraulic retention times (HRTs) after adaptation to microorganisms. The biodegradation of CA was disturbed at low pH operation, while the activity of microorganisms recovered again after pH adjustment to neutral condition. Ibuprofen (IBP) degraded under neutral and acidic conditions. Removals of IBP and CA were zero-order and first-order reactions under high and low initial concentrations, respectively. Carbamazepine and diclofenac were not degraded regardless of HRTs and pH.     

上海某城市污水处理厂污水中药物和个人护理用品(PPCPs)的调查研究

通过两次采集上海某大型污水处理厂的水样,采用超高效液相色谱-串联质谱(UPLC-M S/MS)技术对水样中的94种典型药物和个人护理用品(PPCPs)进行分析,并初步分析了污水处理工艺对典型药物的处理效果.结果显示,该厂污水中有咖啡因、布洛芬、酮洛芬、双氯酚酸、氧氟沙星、睾酮、诺龙、磺胺吡啶、磺胺甲恶唑、甲砜霉素、氟甲砜霉素、氯贝酸、磺胺二甲基嘧啶、磺胺间甲氧嘧啶、氯霉素和诺龙等15种药物被检出和定量.初沉出水中药物总浓度为8 643～10 481 ng·L1,主要为咖啡因,出厂水中药物总浓度为1 005 ～1 076 ng·L1.其中,磺胺二甲基嘧啶、甲砜霉素和氟甲砜霉素在相关报道中较少进行检测或没有检出.磺胺二甲基嘧啶、磺胺间甲氧嘧啶、氯霉素和诺龙4种药物经生化反应池(A/A/O)和二沉池处理之后未检出.以A/A/O为核心技术的污水处理工艺对咖啡因、氯霉素、甲砜霉素和诺龙等药物处理效率较好(85％～99％),但对大部分药物处理效果并不显著.     

城市污水处理厂出水中的药品和个人护理品

药品和个人护理品(PPCPs)是近年来受到环境界普遍关注、具有潜在生态风险的新型有机微污染物.城市污水处理厂(STPs)出水排放是PPCPs向环境迁移最重要的途径,而控制PPCPs随STPs出水排放则是控制PPCPs环境影响的关键.本文分类综述了抗生素、消炎止痛药物、精神类药物、β受体拮抗剂、环境雌激素、调血脂药物、合成麝香、其它类等PPCPs的药理与功能、分类、应用现状和生态毒性,重点总结了1998～2012年间全球STPs出水中频繁检出的典型PPCPs及其最高浓度,为开展STPs排放控制研究提供依据.最后,展望了本领域的未来研究方向与发展趋势.     

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7,利用HLB固相萃取柱对水样中PPCPs进行富集,以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相,甲醇和含0.5 mmol·L^-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱,采用多反应监测的质谱扫描模式(MRM)分析测定.26种PPCPs的检出限为0.007—1.78 ng·L^-1,定量限为0.02—5.68 ng·L^-1,回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度,结果表明,地表水中PPCPs的含量普遍高于地下水,磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高,检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L^-1.     

长三角一体化示范区青浦区水环境中22种PPCPs的多介质分布特征及风险评估

采集了长三角一体化示范区青浦区(包括太浦河、金泽水库周边和青西郊野公园)的25个采样点的50个表层水体和沉积物样品,利用高效液相色谱串联质谱(HPLC/MS-MS)分析了样品中的22种药物与个人护理品(PPCPs),详细分析了研究区域目标PPCPs的分布特征、来源和影响因素,并利用商值法对目标PPCPs的生态风险和健康...     

污水处理厂进出水及其受纳水体中典型PPCPs的污染特征

以对乙酰氨基酚为目标物,利用固相萃取(SPE)-高效液相色谱(HPLC)法测定了该药物在泰安市污水处理厂进出水和地表水体中的含量。结果表明,对乙酰氨基酚在污水处理厂进水中均被检出,质量浓度为0.9~238μg/L,表明生活污水为污水处理厂该药物活性成分的来源,出水中质量浓度为ND~8.3μg/L,去除率较高,其中生物降解是主要的降解机制。在泮河中的质量浓度为ND~3.59μg/L,与国内外其他地表水体相比,处于同一个数量级,且污水厂排水口下游水体中目标物浓度高于上游,反映出污水处理厂排放可能是其受纳水体中PPCPs的主要来源之一。     

典型药物污染物的SPE-UPLC-MS-MS检测方法

采用固相萃取-高效液相色谱-串联质谱法(SPE-UPLC-MS-MS)测定自然水体中的10种典型药物污染。比较了2种萃取柱HLB和C18的富集效果,并对水样pH、萃取柱的淋洗溶剂及水样体积进行了优化。结果表明,采用HLB小柱进行富集净化,水样体积为500 mL,调节pH=3.0,95%甲醇洗脱,在0~200μg/L范围内10种药物的标准曲线线性关系良好(r≥0.999),方法检出限0.5~2.0 ng/L,精密度高(RSD10%),加标回收率为64.3%~100.7%。经过对太湖和某污水厂排水口水样的测试,表明该方法适用于自然水体药物的快速检测,同时大部分药物被检出,说明选择的10种目标药物及建立的检测方法对研究中国水体药物污染具有一定的参考价值。