超高效液相色谱-串联质谱同步检测艾比湖中14种抗生素

采用超高效液相色谱-串联质谱法(UPLC-MS/MS),建立了同时检测水样中三类共计14种抗生素的分析方法。水样经HLB小柱萃取富集后,用10%甲醇含0.1%的甲酸溶液定容,以高效液相色谱-串联质谱对目标物进行分析。在最优实验条件下,14种抗生素的线性范围为1.0~500μg/L,相关系数均大于0.99,方法的检出限为0.30~1.23 ng/L。将建立的方法应用于检测艾比湖湖水中14种抗生素的残留分析,结果表明:14种抗生素中共检测出12种,其中氧氟沙星、洛美沙星、环丙沙星、土霉素的检出率为100%,洛美沙星的浓度最高。     

五氟苄基羟胺衍生与GC/MS联用分析大气中的单羰基化合物和多羰基化合物

利用涂布五氟苄基羟胺（PFBHA）的Tenax-TA作为固体吸附剂,采取主动采样的方式采集大气中羰基化合物,再经溶剂洗脱和氮吹浓缩后用气相色谱/质谱（GC/MS）分析,成功检测到14种单羰基化合物和2种二羰基化合物（乙二醛与甲基乙二醛）.研究表明：在吸附剂的装载量为50mg的前提下,当衍生剂的涂布量为260nmol,采集流速为50mL·min^-1时,采集效果最佳.羰基化合物的检测限、平行样的相对标准偏差和样品的加标回收率范围分别为0.54～3.83ng·m^-3、1.0%～14.2%、89.2%～113.8%.该方法在实际大气样品中合适的采样时间为0.5～8.0h.利用此法对上海市宝山区大气中羰基化合物进行了检测,成功检测到16种羰基化合物,且具有明显的日变化趋势.     

超高效液相/串联质谱法测定水中苯甲酰脲类农药残留

建立了固相萃取(SPE)-超高效液相色谱/大气压化学电离源/三重四极杆串联质谱(UPLC-MS/MS)同时测定水中7种苯甲酰脲类杀虫剂残留的方法。过滤后的样品经HLB固相萃取柱富集净化后,目标化合物经10 mL二氯甲烷洗脱并浓缩,1 mL甲醇定容后,采用BEH C18柱,以水(5 mmol/L乙酸铵)-乙腈作为流动相进行梯度洗脱,采用串联质谱作为检测器进行检测。7种苯甲酰脲类杀虫剂在相关线性范围内线性良好(r=0.999 1～0.999 5),回收率为71.8%～114%,相对标准偏差为3.3%～18.8%,方法检出限为7.0～16.0 ng/L。该方法快速,灵敏度高,适用于测定水体中7种苯甲酰脲类杀虫剂的残留。     

螯合技术深度处理焦化废水

分别采用普通氧化混凝法以及螯合技术综合法对某钢铁集团公司焦化厂焦化废水生化处理后出水进行深度处理。使用气相色谱-质谱(GC-MS)联用仪检测分析了生化处理废水以及两种深度处理技术处理后废水的有机污染物组成。研究结果表明,该螯合技术比普通氧化混凝技术更有效地去除焦化废水中大量的含氨氮、酚、氰、吡啶、硫化物、喹啉等有毒有害的有机污染物,特别是一些无法被氧化降解的杂环化合物及衍生物。     

静态液相微萃取-气质联用测定烷基酚方法优化

采用静态液相微萃取前处理方法与气相色谱—质谱联用技术相结合对水样中烷基酚测定方法进行优化。     

理化因素及感染复数对噬菌体MS2活性的影响

噬菌体MS2作为潜在的水中肠道病毒指示生物,已逐渐成为回用水微生物学安全评价指标的主要研究方向之一。测定了温度、pH值、紫外线和感染复数对噬菌体MS2活性的影响。结果表明:噬菌体MS2在70℃时5 min内即会全部失活,在pH值4～10的范围内均可稳定存在,在短波紫外线照射下25 min内即可失活;噬菌体MS2感染其宿主大肠杆菌的最佳感染复数为1。     

固相萃取-气相色谱/质谱法同时测定海水中9种硝基苯类化合物

建立了固相萃取-气相色谱/质谱(GC/MS)同时测定海水中9种硝基苯类化合物的分析方法。海水样品经Oa-sisHLB固相萃取小柱萃取富集,正己烷/丙酮洗脱,采用GC/MS进行定性定量,线性响应良好,基体干扰小,方法检出限在0.03～0.10μg/L(按采样1 L水计),添加回收率在72.8%～116%,精密度为1.2%～5.4%,并利用该方法对广西近岸海域6个点位实际海水样品进行了监测。该方法可以同时满足海水中9种硝基苯类化合物的测定。     

Determination of Acaricide Residues in Saudi Arabian Honey and Beeswax Using Solid Phase Extraction and Gas Chromatography

Determination of acaricide residues of flumethrin, tau-fluvalinate, coumaphos, and amitraz in honey and beeswax was carried out using a rapid extraction method utilizing C-18 SPE cartridges and an analytical method utilizing GC with ECD, NPD, and MSD detectors for the four acaricides. Recovery percentages from the extraction method ranged from 90–102%, while the minimum detection levels ranged from 0.01–0.05 mg/kg for the acaricides. Nine of the 21 analyzed samples were found to be contaminated with the acaricides tau-fluvalinate and coumaphos. Neither flumethrin nor amitraz was detected in any of the honey or wax samples. Coumaphos was found only in honey samples in which two samples exceeded the tolerance levels set by EPA and EC regulations. It has not been detected in beeswax. Five honey samples and eight beeswax samples were found to be contaminated with tau-fluvalinate. One of the wax samples was contaminated with a relatively high residue of tau-fluvalinate and contained above 10 mg/kg.     

冀西北典型北方小城镇污水处理厂中抗生素的分布和去除

抗生素在环境中作为一种新型污染物,是目前污水处理厂中重要的污染物之一.为考察小城镇污水处理厂对抗生素的去除效果,选择3种典型小城镇污水处理工艺(CASS、A~2/O及Orbal氧化沟工艺),研究了4种四环素类、3种β-内酰胺类、4种大环内酯类、3种喹诺酮类和2种磺胺类在进出水中的浓度分布、去除情况以及不同工艺抗生素去除效率,并对抗生素浓度与水质常规指标的相关性进行分析.结果表明,所研究的污水处理厂中氧氟沙星和诺氟沙星为主要抗生素,并且去除效果较好.5个污水处理厂运行情况良好,CASS工艺和Orbal氧化沟工艺对大部分抗生素的去除效果比A~2/O工艺好,抗生素去除率均能达到60%以上.同时,发现CASS工艺和A~2/O工艺对β-内酰胺类(氨苄西林、青霉素)、喹诺酮类(恩诺沙星、氧氟沙星和诺氟沙星)和大环内酯类(克拉霉素)的去除效果最好,Orbal氧化沟工艺对四环素类(四环素、土霉素)和磺胺类(磺胺嘧啶)的去除效果最好.将抗生素浓度和水质基本参数(NH_4~+-N、TN、COD、pH等)进行相关性分析后,发现抗生素浓度与水质基本参数NH_4~+-N、COD呈一定正相关,污染物浓度越高,红霉素(EM)、罗红霉素(ROX)、差向四环素盐酸盐(ETC)、克拉霉素(CLR)、环丙沙星(CIP)、氧氟沙星(OFX)、差向土霉素(E-OTC)、四环素(TC)、土霉素(OTC)以及诺氟沙星(NOR)的浓度也相对更高,这为确保小城镇污水厂的稳定运行,降低抗生素类污染物的生态风险提供了重要参考.     

Tissue distribution of polychlorinated naphthalenes (PCNs) and non-ortho chlorinated biphenyls (non-ortho CBs) in harbour porpoises (Phocoena phocoena) from Swedish waters

Polychlorinated naphthalenes (PCNs) and non-ortho chlorinated biphenyls (non-ortho CBs) were analysed in blubber, nuchal fat, liver, muscle, kidney and brain of three male harbour porpoises (Phocoena phocoena) from the west coast of Sweden. To estimate spatial variation, PCNs and non-ortho CBs were analysed in six blubber samples collected at different anatomical sites of each animal. Highest wet weight concentrations of ΣPCNs were detected in the lipid rich tissues (blubber and nuchal fat) and liver (520–730 and 520 pg/g, respectively) and lowest in brain (22 pg/g). TetraCNs were most abundant in muscle, kidney and brain, while the hexaCNs were most abundant in the lipid rich tissues and liver. The highest lipid weight concentration recorded (11 ng/g) was for the hexaCN congeners no. 66/67 in liver. These coeluting hexaCN congeners accounted for 80–100% of total hexaCNs in all tissues examined.

Concentrations of Σnon-ortho CBs were highest in lipid rich tissues (220–280 pg/g wet weight). Non-ortho CB no. 77 and 169 constituted between 62–86% and 4.9–9.3%, respectively, of total Σnon-ortho CBs. No major variation of Σnon-ortho CB concentrations was found between the six different blubber sites but higher ΣPCN concentrations (wet weight) were found dorsally at the peduncle. Toxic equivalent concentrations (TEQs) showed that non-ortho CB no. 126 was the main contributor to total TEQs in all tissues, except liver in which hexaCN congener nos. 66/67 contributed to about 50% of total TEQs.