城市污水处理厂水样中有机氯农药残留分析

建立了基于HLB固相萃取柱和气相色谱/电子捕获(GC/ECD)分析城市污水中有机氯农药的分析方法,对北京市五大城市污水处理厂———高碑店、北小河、酒仙桥、清河、方庄污水处理厂进出水水样中有机氯农药进行了分析。在5个污水处理厂的水样中共检出了6种有机氯类农药,分别是α-六六六、β-六六六、γ-六六六、δ-六六六、艾氏剂、4,4’-滴滴伊和异狄氏剂,浓度在0.2~76.4ng/L之间。方法对有机氯农药的回收率达到60.93%~141.50%,方法检测限为(0.27~2.90)ng/L。     

校准曲线制备及应用中的一些问题

阐述了校准曲线的制备和应用，标准加入法，空白值参与回归，工作曲线和标准曲线的一些应注意的问题。     

不同功能区表层土中全氟化合物污染指纹及其来源解析

为探究区域功能对其表层土中全氟化合物(perfluorinated compounds,PFCs)污染指纹与含量水平的影响,采用固相萃取分离富集、高效液相色谱-质谱联用与源解析相结合的方法,分析了深圳市公园、居民小区、十字路口、工厂周边4个功能区和城市背景共76份表层土中14种PFCs的含量.结果表明,深圳市表层土总PFCs(ΣPFCs)含量受区域功能影响显著,呈工厂周边(P<0.001)>>十字路口(P<0.01)>>居民小区(P<0.05)>>公园>城市背景的分布.其中工厂周边、居民小区、公园表层土中PFCs呈中链(P<0.05)>>长链>短链的分布,而十字路口则呈中链≈短链(P<0.05)>>长链的分布.同时,以全氟辛烷磺酸、全氟辛酸、全氟十三酸为主要标志物的3个主成分可以解释深圳表层土超过81%的ΣPFCs,十字路口以及电镀、油漆厂周边表层土呈现出较清晰的PFCs污染指纹.     

Occurrence of PCBs and PAHs in an urban soil of Madrid (Spain)

Polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) were analysed in surface soil samples collected in 2001–2002 at an open urban area of Madrid. In order to obtain representative samples, three collection points at the site were chosen. The most abundant PAHs and PCBs were phenanthrene, fluorene, pyrene, chrysene and benzo[a]pyrene and hexa- and heptachlorinated PCBs, respectively. The sum of selected PAHs (13 compounds) and PCBs (15 congeners) averaged 1 and 0.1?µg?g^?1, respectively. PCB levels in winter were 2–10 times higher than summer ones, while seasonal variation for most of PAHs were not observed. Good correlations among all PCBs were found. Five PAHs were also well correlated.     

河水及底质中内分泌干扰物的分析方法研究

使用SDB-XC膜进行萃取,使用多种溶剂依次进行洗脱并收集脱液后进行GC/MS分析测定,从测定结果的准确度和精密度看,本文提出的前处理及分析测定方法对液体及固体中的多种内分泌的测定均可行。     

涂料稀释剂中的有机污染物分析

采用HP-5毛细管柱分离涂料稀释剂中的有机组份，气相色谱-质谱联用技术定性分析涂料稀释剂中的有机组份，FID检测器定量分析，采用面积归一法计算主要成份的体积分数，并对该涂料稀释剂的毒性进行评估。     

水和正已烷中痕量四氯联苯光降解研究

多氯联苯(PCBs)已成为全球性污染物,在人类生存的各种环境因素中,包括空气、水体、土壤、生物体,甚至远离大陆的海洋中已都发现PCBs的存在.自从发现PCBs能吸收190—240nm和280—310nm紫外光以来,人们推断PCBs吸收阳光中的紫外线后的光降解可能是从环境中除去PCBs的一种有效途径.因此对PCBs的光降解     

Comparative study of the linearity and sensitivity of electron capture and flame photometric detectors using a pesticide standard

Abstract

A study was undertaken to compare and evaluate the different types of ⁶³Ni and ³H electron capture (ECD) and flame photometric detectors (FPD) as part of the Canadian Check Sample Program on Pesticide Residue Analysis. Twenty‐seven laboratories were supplied with chlorpyrifos standard solutions for the determination of linear range and minimum detectable amounts (MDA). Each laboratory selected its own operating conditions except for the FPD study. Results for the FPD were compared with standardized flame conditions designed to optimize the exponential factor in the S‐mode. The MDA of the ECDs (pulsed and direct‐current) ranged from 0.09 to 0.17 pg/sec for ⁶³Ni and ³H sources respectively. The corresponding MDA for the linearized ECDs (pulse modulated or constant current) was 0.04 pg/sec and a linear range of 10⁴ or greater with nitrogen as the carried gas. Use of argon/methane and a pulse width of 0.1 usec extended this range to 10⁵ but the sensitivity was not as great as with nitrogen carrier gas. The practical limit of detector sensitivity was found to be instrument dependent depending primarily on the noise level. In the FPD study, operating in the P‐mode gave an average MDA of 5.97 pg/sec and a linear range of 2 x 10³. Similarly, the S‐mode parameters were 81.1 pg/sec and 8 x 10² respectively with an average exponential factor of n 1.8. Attempts to apply optimized detector gas‐flow conditions improved sensitivity and linearity in the S‐mode only.     

Quantification of ionophores in aged poultry litter using liquid chromatography tandem mass spectrometry

Veterinary anticoccidials, biochemically known as ionophores, are widely used in poultry feed at therapeutic levels to treat Coccidiosis and at sub-therapeutic levels for growth- promotion. Commonly used ionophores in the US poultry industry are monensin, salinomycin, lasalocid and narasin. There is an increasing concern regarding the persistence of these anticoccidials in the environment. However, little attention has been directed to methods development for quantitatively measuring ionophores in complex environmental matrices such as poultry litters that are land applied. Here, we describe a rapid and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS)-based method developed for simultaneous quantification of monensin, lasalocid, salinomycin, and narasin in aged poultry litter samples. Results show significant level of monensin (97.8 ± 3.2 μg kg^?1), lasalocid (19.2 ± 6.6 μg kg^?1), salinomycin (70 ± 2.7 μg kg^?1) and narasin (57.3 ± 2.6 μg kg^?1) in poultry litter stored for over three years at < 5°C. Our findings indicate that even after several years of unmanaged storage of poultry litter, ionophores may continue to persist in this matrix, raising the possibility of prolonged release into the environment.     

气相色谱/三重四极杆质谱用于农药多残留的快速分析

本文建立了一种基于三重四极质谱SRM扫描的农药残留快速分析方法.使用15m的色谱柱,有效缩短了整个分析程序的时间.并通过三重四极质谱的多通道快速扫描的特点,有效解决了重叠农药峰检测的问题,在保证色谱峰强度的同时,得到了足够的数据点.整个分析过程采用一针进样,22min内可对包括有机磷农药、有机氯农药、氨基甲酸酯类农药和菊酯类农药(包括溴氰菊酯)在内的超过150种化合物同时进行准确分析.方法准确灵敏,大部分农药的检测下限可达到0.1 ppb,完全满足肯定列表及欧盟对农药残留限量的要求.