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.     

Possibilities and limitations of ecotoxicological testing of chemicals

This study concerns the polycyclic aromatic hydrocarbons (PAH's) emission from gasoline and diesel automobile engines.

The sampling procedure, the extraction and the analytical method are presented. Using the gas chromatography‐mass spectrometry technique it is possible to detect and quantify easily about 15 PAH's. Data obtained on exhaust particles collected from gasoline and diesel automobile engines are presented and discussed.     

Investigation of naphthalene contamination in olive oil from Greece

Abstract

Incidents of using naphthalene in olive orchards as a repellent of olive fly (Bactrocera oleae) have recently been recorded. Naphthalene, the primary ingredient of mothballs, is described to be diluted in plastic bottles and hanged on the trees releasing its characteristic odor which is supposed to repel olive fly. Since naphthalene has been characterized as possibly carcinogenic to humans and animals, it was considered essential to monitor olive oils regarding their potential contamination with this specific pollutant. To this goal, a simple, sensitive and reliable analytical method for the determination of naphthalene in olive oil has been developed. The method involves extraction with ethyl acetate: acetonitrile (1:1) and determination of naphthalene using gas chromatography triple quadrupole mass spectrometry. The method was validated in four fortification levels, 0.005, 0.01, 0.05, and 0.1?mg/kg in accordance with the EU requirements. The obtained results were acceptable as far as validation criteria are concerned, given recoveries between 71% and 87% and RSDs between 5% and 24%. The limit of determination for naphthalene was set at 0.005?mg/kg based on the lowest concentration level being validated with acceptable accuracy. The analytical technique was successfully applied to 75 olive oil samples collected from oil mills in Greece and no positive results of naphthalene were detected.     

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.     

气相色谱-质谱联用测定母乳中合成麝香

建立了凝胶渗透色谱(GPC)柱和硅胶柱净化,气相色谱-质谱(GC/MS)测定母乳中合成麝香的分析方法.实验结果表明:GC/MS在0.01μg.ml-1到1μg.ml-1的浓度范围内对4种常见合成麝香(佳乐麝香HHCB、吐纳麝香AHTN、二甲苯麝香MX和酮麝香MK)均有良好的线性响应,4种合成麝香的基质加标回收率为76%—115%,相对标准偏差为2.8%—7.4%.利用信噪比(5/1)确定该方法的定性检测限,HHCB,AHTN,MX为5ng.g-1脂重,MK为4ng.g-1脂重,定量检测限为定性检测限的2倍.采用上述方法分析了上海母乳样品中合成麝香的浓度和分布特征,发现母乳中普遍存在这4种合成麝香,浓度分别为HHCB92±70;AHTN16±12;MX26±22;MK16±14ng.g-1脂重,与欧美国家的污染水平相比,总体含量偏低.     

气相色谱-质谱联用测定水产品中的合成麝香

利用快速溶剂萃取（ASE）和在线吸附净化,气相色谱-质谱（GC/MS）联用测定水产品中8种合成麝香.以正己烷为萃取溶剂,中性氧化铝为吸附剂,在100℃的温度下对水产品进行萃取.实验结果表明,方法的检测限为0.1—0.5 ng·g-1;在浓度1—80 ng·g-1的范围内,峰面积与样品浓度呈良好线性关系;8种合成麝香的回...     

Primary and secondary organic aerosol in an urban/industrial site: Sources, health implications and the role of plastic enriched waste burning

PM10 samples were collected from an urban/industrial site nearby Athens, where uncontrolled burning activities occur. PAHs, monocarboxylic, dicarboxylic, hydroxycarboxylic and aromatic acids, tracers from BVOC oxidation, biomass burning tracers and bisphenol A were determined. PAH, monocarboxylic acids, biomass burning tracers and bisphenol A were increased during autumn/winter, while BSOA tracers, dicarboxylic- and hydroxycarboxylic acids during summer. Regarding aromatic acids, different sources and formation mechanisms were indicated as benzoic, phthalic and trimellitic acids were peaked during summer whereas p-toluic, isophthalic and terephthalic were more abundant during autumn/winter. The Benzo[a]pyrene-equivalent carcinogenic power, carcinogenic and mutagenic activities were calculated showing significant (p < 0.05) increases during the colder months. Palmitic, succinic and malic acids were the most abundant monocarboxylic, dicarboxylic and hydrocarboxylic acids during the entire sampling period. Isoprene oxidation was the most significant contributor to BSOA as the isoprene-SOA compounds were two times more abundant than the pinene-SOA (13.4 ± 12.3 and 6.1 ± 2.9 ng/m³, respectively). Ozone has significant impact on the formation of many studied compounds showing significant correlations with: isoprene-SOA (r = 0.77), hydrocarboxylic acids (r = 0.69), pinene-SOA (r = 0.63),dicarboxylic acids (r = 0.58), and the sum of phthalic, benzoic and trimellitic acids (r = 0.44). PCA demonstrated five factors that could explain sources including plastic enriched waste burning (30.8%), oxidation of unsaturated fatty acids (23.0%), vehicle missions and cooking (9.2%), biomass burning (7.7%) and oxidation of VOCs (5.8%). The results highlight the significant contribution of plastic waste uncontrolled burning to the overall air quality degradation.     

大气中挥发性有机物在线监测系统

一种新型的监测大气中挥发性有机物（包括含氧挥发性有机物）的在线监测系统被研制,即将超低温冷阱捕集-热解析装置与气相色谱-质谱仪联用.其分析方法是大气样品经除水、除O3后以60 mL·min-1的流速通过温度为-150℃的超低温冷阱捕集5min,然后样品在110℃下解析后进入GC-FID/MS系统进行分析,时间分辨率为1h.系统使用混和标气进行标定.目标化合物定量曲线的R2值为0.9137~0.9998,相对标准偏差(RSD)均小于10%.将系统与相关商业化的VOC在线监测仪器进行比对,对于相同目标化合物进行分析,其相关系数r在0.7412~0.9620之间.     

气相色谱／质谱（GC／MS）联用在我国大气有机污染监测中的应用

概述ＧＣ／ＭＳ联用在我国大气有机污染监测中的应用，介绍大气中有机污染物，如多环芳烃、硝基多环芳烃、多氯二苯并二恶英、多氯二苯并呋喃、碳氢化合物、苯系物、恶臭、有机硫化合物、多组分有机污染物的测定。