广州某黑臭河涌沉积物中的挥发物质组分

在广州市城区内的猎德涌采集了3个采样点中0~10cm深的表层沉积物,通过DVB/CAR/PDMS固相微萃取(SPME)纤维顶空富集,使用气相色谱/质谱联用仪(GC/MS)对其挥发物进行检测分析。在猎德涌的沉积物中共检测出54种挥发物质,包括36种烷烃、2种环烷烃、1种烯烃、2种硫单体、13种带有发香基团的有机物。在3个采样点分别鉴定出19、49、52种挥发物。在下游河段沉积物中检测出的挥发物种类和峰面积都超过上游。由挥发物质的组成可以判断出其主要污染是来源于交通污染和居民的日常生活污染,其中有3种毒性较大的成分:万山麝香、邻苯二甲酸二异丁酯(DIBP)和2,4-二叔丁基苯酚。     

土壤-植物系统重金属形态分析和生物有效性研究进展

介绍了土壤-植物系统中重金属连续提取的形态分析方法研究进展,同时归纳了影响重金属生物有效性的主要因素,如土壤性质、复合污染及根际环境等,并指出了需要解决的问题与今后的发展方向。     

土壤中13种有机氯农药超声波提取方法研究

应用超声波提取江西红壤和南京黄棕壤中的 13种有机氯农药 (α 、β 、γ 和δ HCH ,2 ,4′ DDT ,2 ,4′ DDE ,4 ,4′ DDT ,4 ,4′ DDE ,4 ,4′ DDD ,α endosulfan ,dieldrin ,endrin ,HCB) ,固相萃取柱进行纯化 ,气相色谱进行定量分析 .对不同提取溶剂 (正己烷、二氯甲烷、正己烷和甲醇、正己烷和丙酮、正己烷和二氯甲烷 )、提取时间 (0 .5～ 2h)、提取次数 (1～ 5次 )与提取效率的关系进行了研究 .研究表明以正己烷 甲醇 (4∶1)作为混合提取溶剂 ,超声提取一次 ,提取 2h能取得较高的提取效率 .此技术节省溶剂且提取方法简单 .     

厌氧滤池-膜生物反应器处理垃圾渗滤液不同工艺段中有机氯农药残留的分析

建立了基于HLB固相萃取柱和气相色谱／电子捕获(GC／ECD)分析垃圾渗滤液中有机氯农药的分析方法,对厌氧滤池．膜生物反应器处理垃圾渗滤液不同工艺段水体中有机氯农药的浓度进行了分析．结果表明,应用厌氧滤池．膜生物反应器处理垃圾渗滤液可以有效去除有机氯农药残留,主要去除工艺是厌氧,其中P,P’-DDT厌氧反应的中间体产物是P,P’-DDD,大部分继续转化为其它产物．在所试验的垃圾渗滤液中没有检出DDTs和HCHs以外的其它优先控制有机氯农药．     

固相萃取-LC-MS定性分析微生物呼吸醌方法的建立

以UQ-6,UQ-10和Vitamin K1作为研究对象,建立了固相萃取LC-MS定性分析微生物呼吸甲基萘醌(MK-n(Hz))和泛醌(UQ-n(Hx))的方法,并用此法定性分析了厌氧活性污泥中的微生物呼吸醌,该方法具有选择性强、灵敏度高的优点,是一种非常有效的微生物种群分析方法。     

化学破乳絮凝与SBR二段法处理采油污水的试验研究

采用化学絮凝与 SBR生化联合的二段法工艺对采油污水进行处理 ,采油污水经第一段化学破乳絮凝后 ,CODCr去除率可达 85 %以上 ,油去除率可达 95 %以上 ;第一段处理出水再经第二段 SBR生化处理后可使出水中 CODCr≤ 60 mg/L、BOD≤ 3 0 mg/L、SS<3 0 mg/L、油 <10 mg/L,达到了油田回注水标准和含油污水的国家二级排放标准 ,可实现废水的资源化     

全自动固相萃取-GC-MS/MS法测定水中多氯联苯

采用全自动固相萃取-气相色谱/三重四极杆串联质谱法(SPE-GC-MS/MS)分析水中7种指示性多氯联苯,通过优化测定条件,使PCBs在0.100μg/L～100μg/L范围内线性良好,方法检出限为0.07 ng/L～0.1 ng/L,回收率为72.1%～102%,RSD为5.8%～12.9%。将该方法用于实际水样测定,结果城市污水处理厂的出水中PCBs检出率较高,而废旧电容器封存点周边地表水易受到PCBs的污染。     

Development,validation of QuEChERS-based method for simultaneous determination of multiclass pesticide residue in milk,and evaluation of the matrix effect

Extraction and quantification of pesticide residue from the milk matrix at or below the established maximum residue limit (MRL) is a challenging task for both analytical chemists and the regulatory institutions to take corrective actions for the human health and safety. The main aim of the study is to develop a simple rapid and less expensive QuEChERS extraction and cleanup method for simultaneous analysis of 41 multiclass pesticide residue in milk by gas chromatography-electron capture detector (GC-ECD), followed by confirmation of the residues with gas chromatography-mass spectrometer (GC-MS). Effect of sorbent type, temperature, spiking concentration, matrix effect (ME), measurement uncertainty (MU), inter- and intra-assay repeatability, reproducibility of recovery, and trueness of the results were investigated to validate the effectiveness of the method. Limit of determination (LOD) and limit of quantitation (LOQ) for all the analytes ranged within 0.001–0.02 and 0.002–0.05 µg mL^?1, respectively. The % recovery of all the pesticides ranged between 91.38 and 117.56% with relative standard deviation (RSD) below 2.79%. The MU for all the analytes was ≤29% of respective LOQs, and except for few pesticides, the ME was largely negative. The method fulfilled all the SANTE guidelines and thus can be extended for routine analysis of multiclass pesticide residue in milk.     

青鳉鱼的行为特征提取研究

采用生物行为传感器获取青鳉鱼的行为数据时,青鳉鱼个体差异会导致采集到的原始电信号在时空特性下完全不同。重要的行为特征往往被隐藏在原始信号中,传统的信号处理方法无法实时而有效地提取到这些特征。针对这个问题,观察并记录了暴露实验前后青鳉鱼的行为变化,提出了一种可以高效表征行为特征的直方图统计算法。实验结果表明,该方法能够准确对应人眼观测到的暴露实验前后鱼的行为变化趋势,同时也为后续异常行为识别提供一定的支持和参考。     

An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal care products in environmental waters

• A hydrophilic resin (GCHM) was facile synthesis and characterized. • Average absolute recovery of GCHM (75.6%) performs better than Oasis^® HLB. • Detection limits of method (SPE-UPLC-MS/MS) ranged between 0.03 and 0.6 ng/L. • 22 PPCPs were determined in environmental waters ranging from 0.5 to 1590 ng/L. In this study, a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-co-divinylbenzene), characterized, and applied as a solid-phase extraction (SPE) material. Up to 44 pharmaceuticals and personal care products (PPCPs) belonging to 10 classes were recovered in environmental water samples. Different variables affecting extraction, such as adsorbent amount, sample pH, and loading speed, were optimized. Under optimal conditions, the average absolute recovery of 44 PPCPs was 75.6% using GCHM, indicating a better performance than the commercial Oasis^® HLB. SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated, and the method achieved good linearity (r²>0.991, for all analytes). In addition, the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L. The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River, Huaihe River, and Taihu Lake, 1 groundwater sample from Changzhou in Jiangsu Province, 1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province, China. In these samples, 22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.