SPE-GC-MS/MS法测定水源水中多种有机氯EDCs

采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。     

直接进样-热脱附-GC-MS快速测定大气细颗粒物中有机示踪物

建立了直接进样-热脱附-GC-MS快速测定细颗粒物中甾烷类和藿烷类有机示踪物的方法。经实验条件优化,13种目标化合物的线性回归方程的相关系数均在0.990以上,空白加标回收率为81.4%~102.3%,实际样品加标回收率为79.1%~112.9%,相对标准偏差小于13.2%。当采样体积为24 m~3时,各目标化合物的检出限为0.008~0.084 ng/m~3,方法灵敏度高。利用该方法测定了北京城区采暖季和非采暖季PM2.5实际样品,结果表明:各目标物均有检出,且采暖季的甾烷类和藿烷类化合物的总量均明显高于非采暖季。该方法无需复杂的前处理和有机溶剂,操作简便快捷,在颗粒物中非极性化合物的快速检测方面具有很大的应用价值。     

环境污染物快速检测技术的国内外研究进展

介绍了环境污染物的分类与危害,基于目前国内外不同类型污染物快速检测技术的研究进展,综述了包括离子传感器、气体传感器和生物传感器等在内的化学传感器选择性强、成本低廉、可检测痕量污染物的优势,以及便携式检测设备节省时间、避免样品采集、应用领域广泛的特点,并提出了污染物快速检测技术的未来发展方向。     

Does malaoxon play a role in the geno- and cytotoxic effects of malathion on human choriocarcinoma cells?

This investigation was undertaken to elucidate whether the active metabolite of malathion, malaoxon, has any role in exerting cyto- and genotoxic effects for human choriocarcinoma (JAR) cell line which is an acceptable model for human placental cells. Gas chromatography-mass spectrometry (GC-MS) analysis were separately performed on the cell compartment and supernatant cell culture medium after subjecting the cell line to different malathion concentrations (10–400 μg/mL) and for various incubation periods (0.5 to 24 hours). GC-MS analysis showed that the sonication performed for the disruption of the cells did not cause the chemical change of malathion. The uptake of malathion by the cells was relatively fast. However, the presence of malaoxon, even in trace amounts, could not be confirmed either in samples originating from disrupted cells or in the cell culture medium. Although the hydrolysis of malaoxon occurred in the culture medium, this degradation process could not be counted as a reason for the absence of malaoxon. Since both malathion and malaoxon standard compounds could be accurately detected and distinguished by the applied liquid-liquid extraction and GC-MS methods, one can conclude that, in the case of JAR cells, the parent compound, (i.e. malathion itself) is responsible for the observed in vitro cyto- and genotoxic effects. Our results indicate that the direct toxicity of malathion contributes to the complications of pregnancy observed for environmental malathion exposure.     

Estimation of β-cyfluthrin and imidacloprid in okra fruits and soil by chromatography techniques

Dissipation of β-cyfluthrin and imidacloprid in okra was studied following three applications of a combination formulation of Solomon 300 OD (β-cyfluthrin 9 % + imidacloprid 21 %) @ 60 and 120 g a.i. ha^?1 at 7 days interval. Residues of β-cyfluthrin and imidacloprid in okra were estimated by gas liquid chromatography (GLC) and high performance liquid chromatography (HPLC), respectively. Residues of β-cyfluthrin were confirmed by gas chromatograph–mass spectrometry (GC-MS) and that of imidacloprid by high performance thin layer chromatography (HPTLC). Half-life periods for β-cyfluthrin were found to be 0.91 and 0.68 days whereas for imidacloprid these values were observed to be 0.85 and 0.96 days at single and double the application rates, respectively. Residues of β-cyfluthrin dissipated below its limit of quantification (LOQ) of 0.01 mg kg^?1 after 3 and 5 days at single and double the application dosage, respectively. Similarly, residues of imidacloprid took 5 and 7 days to reach LOQ of 0.01 mg kg^?1, at single and double dosages respectively. Soil samples collected after 15 days of the last application did not show the presence of β-cyfluthrin and imidacloprid at their detection limit of 0.01 mg kg^?1.     

Multiresidue determination of pesticides in tea by gas chromatography-tandem mass spectrometry

An efficient and reliable GC-MS/MS method for the multiresidue determination of pesticides in tea was developed by modifying the Japanese official multiresidue method. Sample preparation was carefully optimized for the efficient removal of coextracted matrix components. The optimal sample preparation procedure involved swelling of the sample in water; extraction with acetonitrile; removal of water by salting-out; and sequential cleanup by ODS, graphitized carbon black/primary secondary amine (GCB/PSA) and silica gel cartridges prior to GC-MS/MS analysis. The recoveries of 162 pesticides from fortified (at 0.01 mg kg^?1) green tea, oolong tea, black tea and matcha (powdered green tea) were mostly (95–98% of the tested pesticides) within the range of 70–120%, with relative standard deviations of <20%. Poor recovery of triazole pesticides was considered to be due to low recovery from the silica gel cartridges. The test solutions obtained by the modified method contained relatively small amounts of pigments, caffeine and other matrix components and were cleaner than those obtained by the original Japanese official multiresidue method. No interfering peaks were observed in the blank chromatograms, indicating the high selectivity of the modified method. The overall results suggest that the developed method is suitable for the quantitative analysis of GC-amenable pesticide residues in tea.     

Analysis of mixed halogenated dibenzo-p-dioxins and dibenzofurans (PXDD/PXDFs) in soil by gas chromatography tandem mass spectrometry (GC-MS/MS)

Mixed halogenated dibenzo-p-dioxins and dibenzofurans (PXDD/PXDFs, X = Br, Cl) are formed through combustion processes, and may be more toxic than their corresponding chlorinated and brominated analogues. With 4600 potential congeners, limited analytical standards, and complex environmental matrices, PXDD/PXDFs present a significant analytical challenge. Gas chromatography tandem mass spectrometry (GC-MS/MS) offers both selectivity and sensitivity through multiple reaction monitoring of unique transitions in a novel approach to PXDD/PXDF congener identification. Method validation was performed through analysis of soil samples obtained from a recycling plant fire. Of the PXDD/PXDFs examined, monobromo-dichlorodibenzofuran was the most prevalent, ranging in concentration from 8.6 ng g⁻¹ to 180 ng g⁻¹. Dibromo-dichlorodibenzo-p-dioxin, a compound of toxicological concern, ranged from 0.41 ng g⁻¹ to 10 ng g⁻¹. Concentrations of PXDD/PXDFs were between 6% and 10% that of the corresponding polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/PCDFs), with the exception of dibromo-dichlorodibenzo-p-dioxin concentrations, which were 36% that of tetrachlorodibenzo-p-dioxins. Higher levels of polybrominated PXDD/PXDFs may indicate a significant bromine source was present during combustion.     

水中佳乐麝香的固相微萃取-气质联机测定方法

采用聚二甲基硅氧烷膜厚100μm的纤维萃取设备,阐述了测定水中HHCB的固相微萃取-气质联机的检测方法。研究发现,对于水中的HHCB来说,温度控制在35℃,萃取时间为40 min,pH值为7.0,可实现HHCB的有效萃取,水中的离子对萃取效率的干扰较小。使用该方法测得上海龙华污水厂原水中HHCB浓度为286 ng/L,虹口区泗塘河水中HHCB浓度低于检测下限。     

Determination of volatile organic sulfur compounds in contaminated groundwater

A practical method for the quantification of total purgeable organic sulfur (POS) in highly contaminated groundwater is described. Volatile organic sulfur compounds (VOSC) are purged from the water samples by a stream of oxygen and combusted. The emerging sulfur dioxide is absorbed in H₂O₂ and converted to sulfate which is quantified by ion chromatography and reported as mass sulfur equivalent. The overall limit of quantification is 0.03 mg l⁻¹. The content of POS is balanced with the total VOSC determined by GC-AED after liquid–liquid extraction. Separate determination of the non-volatile organic sulfur compounds by direct combustion of the water sample and adsorption to charcoal yielded a mass balance of the total sulfur content. Semi-quantitative GC-MS after purge & trap accumulation revealed that the VOSC mixture is composed of C₁–C₄ alkyl sulfides. The implementation of the developed methodology for the quantification of VOSC as potential catalyst poison in a cleaning plant for groundwater contaminated with volatile haloorganics (VOX) is presented.     

气相色谱-质谱法分析饮用水源水中甲基汞

采用自动固相萃取-气质联用法分析饮用水源中的甲基汞,通过巯基棉小柱萃取大体积(5L)水样后,选择离子扫描方式(SIM)进行定量。实验对比国家标准方法具有更好的线性关系,实际操作简单快捷,灵敏度高。3个浓度水平进行加标回收实验,回收率分别大于71.0%、74.4%、76.0%。对10μg/L浓度重复进样6次,相对标准偏差(RSD)为4.8%。该方法检出限可达到3×10-4μg/L,满足饮用水源水中甲基汞标准限值要求。