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Elemental Analysis of Biological Matrices by Laser Ablation High Resolution Inductively Coupled Plasma Mass Spectrometry (LA-HR-ICP-MS) and High Resolution Inductively Coupled Plasma Mass Spectrometry (HR-ICP-MS)Castro, Waleska 03 November 2008 (has links)
The need for elemental analysis of biological matrices such as bone, teeth, and plant matter for sourcing purposes has emerged within the forensic and geochemical laboratories. Trace elemental analyses for the comparison of aterials such as glass by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS has been shown to offer a high degree of discrimination between different manufacturing sources. Unit resolution ICP-MS instruments may suffer from some polyatomic interferences including 40Ar16O+, 40Ar16O1H+, and 40Ca16O+ that affect iron measurement at trace levels. Iron is an important element in the analysis of glass and also of interest for the analysis of several biological matrices. A comparison of the nalytical performance of two different ICP-MS systems for iron analysis in glass for determining the method detection limits (MDLs), accuracy, and precision of the measurement is presented. Acid digestion and laser ablation methods are also compared. Iron polyatomic interferences were reduced or resolved by using dynamic reaction cell and high resolution ICP-MS. MDLs as low as 0.03 ìg g-1 and 0.14 ìg g-1 for laser ablation and solution based analyses respectively were achieved. The use of helium as a carrier gas demonstrated improvement in the detection limits of both iron isotopes (56Fe and 57Fe) in medium resolution for the HR-ICP-MS and with a dynamic reaction cell (DRC) coupled to a quadrupole ICP-MS system. The development and application of robust analytical methods for the quantification of trace elements in biological matrices has lead to a better understanding of the potential utility of these measurements in forensic chemical analyses. Standard reference materials (SRMs) were used in the development of an analytical method using HR-ICP-MS and LA-HR-ICP-MS that was subsequently applied on the analysis of real samples. Bone, teeth and ashed marijuana samples were analyzed with the developed method. Elemental analysis of bone samples from 12 different individuals provided discrimination between individuals, when femur and humerus bones were considered separately. Discrimination of 14 teeth samples based on elemental composition was achieved with the exception of one case where samples from the same individual were not associated with each other. The discrimination of 49 different ashed plant (cannabis)samples was achieved using the developed method.
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Développement de la méthodologie analytique et surveillance des contaminants dans le panier de la ménagère au Liban / Analytical methods development and survey of selected contaminants in a Lebanese food basketBou Khouzam, Rola 12 December 2011 (has links)
L’objectif du travail est d’évaluer le niveau des contaminants (éléments à l’état de traces et pesticides) dans quatre types de produits alimentaires (pain, fromage, végétaux et fruits) et eau potable considérés parmi les produits les plus consommés par les Libanais suivant l’étude du panier de la ménagère faite en 2006. Une méthode analytique pour l’analyse multi élémentaire a été optimisée pour augmenter la sensibilité et réduire les interférences polyatomiques en utilisant la technique de spectrométrie de masse de haute résolution par plasma induit pour la détermination de 20 éléments mineurs et à l’état de trace afin d’évaluer la valeur nutritive et le niveau de contamination. Pour l’analyse des résidus de pesticides, une méthode analytique a été développé pour la détermination des résidus dans des fromages riches en matières grasses (2-25%). La détermination des résidus de pesticides dans le pain, les végétaux et les fruits a été accomplie suivant la méthode QuEChERS. La surveillance du taux des contaminants a été faite sur des échantillons collectés dans des marches de cinq régions géographiques au Liban durant les saisons humide et sèches. / The objective of this work was to evaluate the level of food contaminants, trace elements and pesticides residues, in four types of commodities bread, white cheese, vegetables and fruits, and drinking water considered as the most consumed by the Lebanese population based on the Food Basket Study on 2006. A multielemental method was optimized in terms of sensitivity and inference elimination by using high resolution sector field inductively coupled plasma mass spectrometry (HR ICP/MS) for the determination of 20 minor and trace elements in the selected foods to assess the nutritional contribution and the level of contamination. For pesticides residues analysis, an analytical method was developed for the quantification of residues in cheese (2-25% fat). Bread, vegetables and fruit were analysed according to the QuEChERS method. For the monitoring study, the samples were collected during two seasons, wet and dry, from five geographical regions in Lebanon.
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