Development and assessment of an onsite large volume solid phase extraction (LV-SPE) device for the determination of pharmaceuticals and personal care products (PPCPs) in water

It is essential to determine the occurrence of emerging organic contaminants(EOCs),such as pharmaceuticals and personal care products(PPCPs),in the ambient environment to address growing public concerns.However,such analysis is quite challenging due to the low trace level of such contaminants in water,which therefore requires several litres of water samples.In this study,a large volume solid phase extraction(LV-SPE)device was developed and evaluated for its performance in monitoring PPCPs as an example.Relatively good recoveries and reproducibility were obtained under specific operating conditions:a water sample volume of no more than 20 L,a flow rate not exceeding 120 mL/min,and a methanol elution volume of at least 30 mL.In addition,the results from the onsite enrichment approach using LV-SPE were compared with those from the conventional approach using a standard SPE device in the laboratory for real groundwater samples.Among the eight selected PPCPs(nalidixic acid,carbamazepine,bezafibrate,clofibric acid,sulfadiazine,sulfamethoxypyridazine,sulfamethazine and sulfamonomethoxine),LV-SPE approach detected more target compounds.While the detected concentrations were generally comparable,slightly higher concentrations were observed for carbamazepine,clofibric acid,sulfadiazine and sulfamethazine using the LV-SPE method.The developed LV-SPE device provides an alternative approach for trace analysis of PPCPs and may also be applicable for other emerging organic contaminants.

Detailed analysis of PCBs and PCDD/Fs impurities in a dielectric oil sample （ASKAREL Nr 1740） from an imported transformer in China

Homolog and congener profiles of polychlori- nated biphenyls （PCBs）, polychlorinated dibenzo-p- dioxins （PCDDs） and polychlorinated dibenzofurans （PCDFs） in commercial PCBs formulations are useful information for the source appointment of PCBs contam- ination as well as the risk assessment caused by potential exposure. Dielectric oil （ASKAREL Nr 1740） in an imported transformer found in China was sampled and analyzed by isotope dilution technology using high resolution gas chromatography-high resolution mass spectrometry （HRGC/HRMS）. The detailed homolog and congener profiles of PCBs obtained were compared with those of known Aroclor formulations. High similarity in the homolog profile between the oil sample and Aroclor 1260was found, with the hexachlorinated and hepta- chlorinated biphenyls accounting for more than 80.2% of the total PCBs concentration. Severn indicator PCBs contribute about 30%, while 12 PCB congeners （i.e., # 153, #143, #168, #180, #149, #165, #138, #170, #190, #187, #174, #181） account for more than 50% of the total PCB concentrations. Total concentration ofPCDDs, PCDFs and dioxin-like PCBs （DL-PCBs） was found to be 740 ng TEQ/g, of which 620 ng TEQ/g came from DL-PCBs. The contribution of PCDDs to the total TEQ was neglectable. The concentration of PCDFs homologs follows the order of OCDF 〉 HxCDFs 〉 HpCDFs 〉 PeCDFs 〉 TeCDFs, which is in consistence with the previous study on Aroclor 1260. Three DL-PCBs congeners （i.e., #118, #156, #157） accounted for 77% of the total concentration of DL-PCBs, also they contribute 72% in the TEQ caused by DL-PCBs.

Determination of persistent organic pollutants by gas chromatography/laser multiphoton ionization/time-of-flight mass spectrometry

An authentic mixture of polychlorinated biphenyls was measured using a short wide-bore capillary column for the group separation of major components present in an actual sample of Kanechlor. The limits of detection were improved by ca. 2 fold in comparison with those obtained using a conventional capillary column, since the retention time was reduced and the amount of analytes introduced into the mass spectrometer per unit time could be increased. On the other hand, surface-water and sediment samples containing polycyclic aromatic hydrocarbons （PAHs） were collected from the river located in the vicinity of a waste water treatment plant. Even acenaphthylene, a minor component of the mixture could be measured for the sediment sample, and the concentra- tions were determined for several heavy PAHs. As demonstrated, a technique involving laser multiphoton ionization/time-of-flight mass spectrometry was useful as a sensitive and selective analytical tool for the trace analysis of persistent organic pollutants in an environmental sample.