Removal of pesticides from water samples by adsorption with fatty acids supported on barium sulphate

Oleic or linoleic acid supported on barium sulphate was used to remove atrazine and terbuthylazine in the range of 0.1–2.0 μg/L using spiked water samples. The sorption of atrazine depends on the stirring time and the best value is 150 min. Terbuthylazine is removed well with a stirring time of 60 min and its adsorption is about 90%. Detection of the residual pesticide in treated waters, after solid phase extraction (SPE), was carried out by GC‐MS operating in selected ion monitoring (SIM) using a calibration curve by direct injection of standard solutions of herbicide.     

Analyses of phenolic compounds occurring in olive oil mill wastewaters by GC–MS

Phenolic compounds in olive oil mill wastewaters were analysed by HRGC–MS after extracting the acidified solution with ethyl acetate and derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide. Both simple and complex phenols were detected with the latter being the most abundant. 1,2-dihydroxybenzene (catechol), p-hydroxyphenyl ethanol (tyrosol), 3,4-dihydroxyphenyl ethanol (hydroxytyrosol) and 4-hydroxy-3-methoxyphenyl ethanol (homovanillyl alcohol) predominated among the simple phenols using a gas chromatograph coupled with a mass selective detector.     

Standard purity and response factors of perfluorinated compounds

It has been reported that the relative response factors of isotopically labeled standards and unlabeled standards of the same perfluorinated compounds could be different. Individual (100 ng mL^?1) solutions of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) were analyzed using high-performance liquid chromatography tandem mass-spectrometry under negative-ion electrospray to detect any impurities present down to 0.5%–0.1% relative to the major component. Purity of the standards ranged from approximately 86% to ≥ 97%. Standard solutions of unlabeled and isotopically labeled materials were analyzed to compare the response factors of isotopically labeled analytes versus their nonlabeled counterparts in three different matrices at equivalent concentrations: organic solvent (methanol), serum extract, and water present individually and concurrently. Not all labeled analytes have the same response factor as their nonlabeled complement, and in at least one case the matrix in which the standard is present may cause significant suppression of response. Standard solutions of electrochemical fluorination produced PFOA and PFOS were quantified under multiple reaction monitoring mode, using calibration curves prepared from standards consisting primarily of linear standards only. The use of linear only standards may cause under-prediction of concentrations, and that the working range of these standards may be limited.     

Evaluation of pesticides multiresidue contamination of khat leaves from Jazan region,Kingdome Saudi Arabia,using solid-phase extraction – gas chromatography/mass spectrometry

The habit of khat chewing is widespread with a deep-rooted sociocultural tradition in these regions and as such poses a public health problem. The use of pesticides is considered to be indispensable practice for the production of adequate food supply for the increasing demands by the global population and for control of insect-borne diseases. Thus, contamination of the environment with pesticides and entry of these chemicals into the food chain is unavoidable especially in developing countries. The main objective of our current study was to assess pesticide pollution of khat leaves (unknown origin) obtained while being smuggled into the Kingdom of Saudi Arabia and to be used in Jazan area. A total of 120 khat leaf samples were extracted using solid-phase extraction followed by gas chromatography/mass spectrometry analysis for the presence of 69 standard pesticides using an internal standard, tiphenyl phosphate. No pesticide residues were detected in all the studied samples. These data as preliminary and more experiments need to be performed to confirm our present findings. Routine monitoring of the pesticide residues is important for the prevention, control, and reduction of environmental pollution and also for legal decisions to minimize health risks.     

超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0μg·L-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.     

液相色谱-串联质谱法同时测定污水中10种精神活性物质

建立了采用液相色谱-串联质谱法(LC-MS/MS)同时测定污水中10种精神活性物质的分析方法。污水样品经甲酸与甲酸铵调节pH后,加入氘代内标混匀,离心并过滤膜后可直接上样分析。研究表明,在1~250 ng/L的线性范围内,10种精神活性物质的线性相关系数均大于0.992,定量限均低于0.5 ng/L。在3个加标水平下,10种精神活性物质的加标回收率为87.2%~114%,相对标准偏差为0.53%~3.60%(n=3)。将该方法应用于某区域10份生活污水样品的检测,在3份水样中检出吗啡、甲基苯丙胺、氯胺酮等精神活性物质,对应的质量浓度范围分别为3.41~9.55、0.90~1.63、1.06~1.78 ng/L。与经固相萃取前处理后的分析方法相比,该方法可在10 min内完成分离和检测的全过程,具有简单、快速、节约的优点,可用于污水样品中10种痕量水平精神活性物质的定量分析。     

GC/MS法测定润滑油基础油中多环芳烃

对润滑油基础油中多环芳烃的气相色谱/质谱(GC/MS)测定方法进行了研究,探讨了样品的提取,固相萃取柱净化等前处理方法,同时也对仪器测定条件进行了优化.结果表明,在检测润滑油基础油中多环芳烃时,经优化的GC/MS法的加标回收率和精密度均达到较满意的水平.     

用Ames试验检测水源水和自来水中的遗传毒性

用微伤寒沙门氏菌／哺乳动物微粒体酶系的Ａｍａｅｓ试验，研究了不同季节物水源水及管网自来水中的遗传毒性，以ＸＡＤ２树脂为吸附剂，以丙酮－甲醇的混合液为洗脱液，浓率水样中的有机物，并对部分阳性水样进行有机成分的定性分析。结果发现：１３个水样中有７个样品在淡需要代谢活化系统Ｓ９的情况下，可诱导鼠伤寒沙门氏菌碱基移码型菌株的回复突变；不同水样在不同季节不同的诱导作用；同时通过ＧＣ／ＭＳ方法分析，发现阳性水     

吹扫捕集与气相色谱-质谱联用测定饮用水和地表水中挥发性有机污染物

报道了Trap I(VOCARB 4000)柱捕集水中挥发性有机污染物的性能和条件,建立了吹扫捕集和气相色谱-质谱联用测定饮用水和地表水样中25种挥发性有机污染物的分析方法.水样的加标回收率在90%～110%之间,最低检测限在0.04～0.85μg/L之间,20μg/L的挥发性有机物标准溶液经重复6次测定,其相对标准偏差基本小于5.0%.该方法已成功地运用于饮用水和地表水中挥发性有机污染物的测定,结果令人满意.     

电感耦合等离子体质谱法在环境监测中的应用

针对ICP-MS技术的使用特点及其近年来在环境监测领域的应用进行综合阐述，并对ICP-MS技术的发展前景作出简单的评述。