松花江水中13种内分泌干扰物的初步调查

用固相萃取(SPE)/高效液相色谱法(HPLC)同时测定了松花江水中的13种典型内分泌干扰物(EDCs).结果表明,哈尔滨段江水中雌三醇(E3)、雌二醇(E2)、雌酮(E1)、乙炔雌醇(EE2)及乙烯雌酚(DES)5种雌激素物质的浓度普遍较高.最高可达66 ng·L-1;酞酸二甲酯(DMP)、酞酸二乙酯(DEP)、酞酸二正丁酯(DnBP)及酞酸二(2-乙基己基)酯(DEHP)4种酞酸酯丰度最大,其中DnBP浓度最高可达330μg·L-1;4-正壬基酚(4-n-NP),带支链的对壬基酚(NP)及4-叔-辛基酚(4-t-OP)3种烷基酚的浓度范围为25-1261 ng·L-1;双酚A(BPA)浓度变化较小,保持在20-50 ng·L-1之间.经与相关报道比较,初步认为松花江水中雌激素类物质及酞酸酯污染较为严重,应当引起有关部门的警惕.     

固相萃取-高效液相色谱法测定海水中多环芳烃

针对环境中常见且对人体危害极大的USEPA优先控制污染物多环芳烃(PAHs)在海水中的监测方法进行研究.以国家标准分析方法和美国环保局分析方法为基础,采用固相萃取-高效液相色谱法来测定.探讨了各条件对测定的影响,经过固相萃取,七种PAHs在反相高效液相色谱中有很好的分离效果,满意的回收率,方法简便,具有良好的应用前景.     

固相萃取-超高压液相色谱-串联质谱法测定海水中16种磺胺类抗生素残留

利用固相萃取前处理方法,净化和富集海水中的16种磺胺类抗生素,采用超高压液相色谱-串联质谱法进行定性和定量检测,建立了完整的海水中磺胺类抗生素的检测方法,并对质谱条件、液相条件和固相萃取条件进行了优化。实验结果表明,16种磺胺类抗生素在0.1～100μg/L质量浓度范围内线性良好,相关系数均可以达到0.996以上,方法检出限为0.3~1.1 ng/L。对水样进行高、中、低3个质量浓度的加标回收实验,回收率分别为82.3%~125.7%,73.3%~125.1%和75.2%~119.2%,相对标准偏差为2.4%~12.0%。该方法具有操作简便、重现性好、灵敏度高的优点,可用于海水中磺胺类抗生素的监测分析。     

多壁碳纳米管固相萃取—高效液相色谱法测定水中7种三唑类农药残留

应用多壁碳纳米管自制固相萃取柱富集、净化,以乙腈-水为流动相,用乙酸乙酯洗脱,高效液相色谱进行分析检测,建立了环境水样中7种三唑类农药残留分析的方法。结果表明,在0.05~10.00mg/L线性范围内,方法检出限为0.000 9~0.047 7mg/L;农药的加标水平在0.25~1.00mg/L时,加标回收率为72.28%~106.60%,相对标准偏差为1.12%~9.73%。该方法操作简单,定性、定量准确,是对水样中三唑类农药残留液相色谱分析较理想的一种方法。     

Determination of biocides and pesticides by on-line solid phase extraction coupled with mass spectrometry and their behaviour in wastewater and surface water

This study focused on the input of hydrophilic biocides into the aquatic environment and on the efficiency of their removal in conventional wastewater treatment by a mass flux analysis. A fully automated method consisting of on-line solid phase extraction coupled to LC-ESI-MS/MS was developed and validated for the simultaneous trace determination of different biocidal compounds (1,2-benzisothiazoline-3-one (BIT), 3-Iodo-2-propynylbutyl-carbamate (IPBC), irgarol 1051 and 2-N-octyl-4-isothiazolinone (octhilinone, OIT), carbendazim, diazinon, diuron, isoproturon, mecoprop, terbutryn and terbutylazine) and pharmaceuticals (diclofenac and sulfamethoxazole) in wastewater and surface water. In the tertiary effluent, the highest average concentrations were determined for mecoprop (1010 ng/L) which was at comparable levels as the pharmaceuticals diclofenac (690 ng/L) and sulfamethoxazole (140 ng/L) but 1-2 orders of magnitude higher than the other biocidal compounds. Average eliminations for all compounds were usually below 50%. During rain events, increased residual amounts of biocidal contaminants are discharged to receiving surface waters.     

Relevance study of bare and coated zero valent iron nanoparticles for lindane degradation from its by-product monitorization

Zero-valent iron nanoparticles (NZVI) as well as polymer–stabilized nanoparticles were synthesized and used for lindane (γ-hexachlorocyclohexane) degradation in aqueous solution. To study the effectiveness of the different coated nanoparticles, simple and rapid analytical methods have been developed to measure and to detect lindane and its by-products. For the monitorization of lindane degradation solid-phase extraction (SPE) was used, while volatile by-products formation measurement was carried out by headspace-solid phase microextraction (HS–SPME) followed by GC/MS. The SPE–GC/MS method provides low detection limits (0.2 μg L⁻¹), high recovery (above 95%) and it is a valuable tool for kinetic studies of the degradation process for each polymer used, while HS–SPME–GC/MS has proved to be an effective tool for the extraction and evaluation of volatile degradation by-products.     

SPE-HPLC法测定固体废物浸出液中苯酚类物质

选择Agilent Bond Elut Plexa作为固相萃取柱,结合高效液相色谱测定固体废物浸出液中12种苯酚类化合物,通过试验优化条件,使目标物在0.100 mg/L~10.0 mg/L范围内线性良好,方法检出限在0.004μg/L~0.068μg/L之间,3个质量浓度水平加标回收率为78.0%~105%,测定6次结果的RSD为0.7%~5.0%。将该方法用于测定江苏省某工业园区污水处理企业5个废水处理污泥样品,结果 2,4,6-三氯苯酚和2,4-二硝基苯酚检出。     

超高效液相色谱三重四级杆质谱联用法测定水中喹诺酮类抗生素

采用固相萃取-超高效液相色谱三重四级杆质谱联用法同时测定水中环丙沙星、氧氟沙星、恩诺沙星、洛美沙星、诺氟沙星等5种喹诺酮类抗生素,优化了前处理和分离检测条件。5种目标化合物在6.5 min内完成分析,在1.00 μg/L～100 μg/L范围内线性良好,方法检出限为0.3 ng/L～1.0 ng/L,空白和实际水样加标回收率为81.5%～116%,平行测定的RSD为6.0%～14.1%。     

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。     

2,4-二硝基苯肼衍生高效液相色谱法测定水中乙醛、丙烯醛

采用2,4-二硝基苯肼高效液相色谱法测定水中乙醛、丙烯醛,方法干扰少,精密度高,检出限达到1μg/L。