Determination of selected elements in canned food sold in Jordan markets.

In this study, the concentrations of seven heavy metals including As, Cd, Cr, Cu, Ni, Pb, and Zn in imported canned food samples of different brands including tuna, beef, sardines, and mushroom were determined. Samples were collected from popular Jordanian market, Irbid city, Northern Jordan (44 samples of each type). The metal concentrations in canned food samples were found to be in the range of 1.85-4.50 µg/g for As, 0.42-0.58 µg/g for Cd, 0.47-1.67 µg/g for Cr, 0.73-0.90 µg/g for Cu, 1.08-2.77 µg/g for Ni, 2.5-3.0 µg/g for Pb, and 0.43-2.25 µg/g for Zn. Results revealed that As and Pb have the highest concentrations in all samples analyzed, whereas, the lowest concentrations obtained were in Cd. For example, in canned sardine, the mean concentrations of heavy metals are 0.43 µg/g for Zn, 2.50 µg/g for Pb, 1.74 µg/g for Ni, 0.80 µg/g for Cu, 0.47 µg/g for Cr, 0.42 µg/g for Cd, and 1.85 µg/g for As. Whereas, the mean concentrations in canned tuna were 3.48 µg/g for As, 0.47 µg/g for Cd, 0.53 µg/g for Cr, 0.73 µg/g for Cu, 2.77 µg/g for Ni, 2.80 µg/g for Pb, and 1.63 µg/g for Zn. The results of this study indicated that the concentration of the tested elements including As, Cd, Cr, Ni, and Pb in canned food samples sold in Jordanian markets exceeded the permissible limits set by health organizations such as FAO/WHO. The results were compared with the literature values.

Determination of heavy metals in canned fruits and vegetables sold in Jordan market.

In this study, the concentrations of selected heavy metals including Pb, Zn, Cr, Ni, Cu, As, and Cd in different brands of canned vegetables and fruits including canned tomato sauce (ketchup), canned green beans, canned whole carrots, and canned juice (pineapple) imported to Jordanian market were determined by acid digestion and atomic absorption spectroscopy. Samples were collected from popular Jordanian markets, Irbid city, Northern Jordan (11 samples of each type). The metal concentrations in the samples analyzed were found to be in the range of 2.6-3.0 mg/kg for Pb, 0.50-0.60 mg/kg for Cd, 2.50-5.10 mg/kg for As, 0.84-0.91 mg/kg for Cu, 0.32-3.02 mg/kg for Zn, 0.66-1.71 mg/kg for Cr, and 0.97-2.94 mg/kg for Ni. The results obtained showed that Pb and As have the highest concentrations in the most of samples analyzed, whereas, the lowest concentrations obtained were mainly in Cd. For example, in canned tomato sauce, the average concentrations of heavy metals are 3.50 mg/kg for As, 0.50 mg/kg for Cd, 0.66 mg/kg for Cr, 0.89 mg/kg for Cu, 1.15 mg/kg for Ni, 2.95 mg/kg for Pb, and 1.02 mg/kg for Zn. The results of this study reveal that the concentration of some toxic heavy metals (Pb, Cr, Ni, As, and Cd) in canned vegetable and fruit samples being sold in Jordanian markets exceeded the permissible limits set by different health organizations.

Mixed-mode acrylamide-based continuous beds bearing tert-butyl groups for capillary electrochromatography synthesized via complexation of N-tert-butylacrylamide with a water-soluble cyclodextrin. Part I: Retention properties.

With the aim to improve the understanding of morphology and efficiency properties, we investigate in this series the impact of the complex formation constant of the hydrophobic monomer with respect to statistically methylated-ß-cyclodextrin (Me-ß-CD) on the electrochromatographic properties of highly crosslinked amphiphilic mixed-mode acrylamide-based monolithic stationary phases. Based on our previous work on amphiphilic mixed-mode monolithic stationary phases for capillary electrochromatography (CEC) using N-(1-adamantyl)acrylamide (Ad-AAm) as hydrophobic monomer that forms an extremely strong water-soluble inclusion complex with Me-ß-CD, we now selected N-tert-butylacrylamide (NTBA) as hydrophobic monomer forming an inclusion complex with Me-ß-CD with a much lower value of the formation constant. Mixed-mode monolithic stationary phases are synthesized by in-situ free radical copolymerization of cyclodextrin-solubilized N-tert-butylacrylamide, a water soluble crosslinker (piperazinediacrylamide), a hydrophilic neutral monomer (methacrylamide), and a negatively charged monomer (vinylsulfonic acid) in aqueous medium in bind silane pre-treated fused silica capillaries. The synthesized monolithic stationary phases have both hydrophobic and hydrophilic moieties and can be employed in the reversed-phase mode, in the normal-phase mode, in a mixed-mode or in the hydrophilic interaction liquid chromatography (HILIC) mode (depending on the composition of the mobile phase and on the properties of the solute). Morphology and retention properties of this new type of stationary phase are compared to those reported in our previous series. With a homologues series of alkylphenones it is confirmed that the hydrophobicity (methylene selectivity αmeth) of the stationary phase is strongly dependent on the type of hydrophobic monomer employed. The studies reveal a significant influence of the formation constant of the involved host-guest inclusion complex on the morphology (i.e., the domain size) of the produced monoliths.

Elucidation of the Enantiodiscrimination Properties of a Nonracemic Chiral Alignment Medium through Gel-based Capillary Electrochromatography: Separation of the Mefloquine Stereoisomers.

Enantiodiscrimination and enantioseparation are two highly important processes in chemistry, often performed by using NMR spectroscopy and chromatography. For a better understanding of the mechanistic details, the same system should be studied by both methods. In addition, isotropic and anisotropic NMR parameters should be obtained, the latter using alignment media so that residual dipolar couplings and chemical-shift anisotropies can be measured. Consequently, a chiral alignment medium was used for the first time in chiral gel-based capillary electrochromatography with the four stereoisomers of the antimalaria drug mefloquine as test compounds. Chromatographic data verify that enantiodiscrimination obtained with this alignment gel is caused by differences in the equilibrium constants related to associate formation. Hence, the chromatographic separation provides physicochemical data that form a basis for the understanding and optimization of alignment processes, and vice versa.

Adamantyl-group containing mixed-mode acrylamide-based continuous beds for capillary electrochromatography. Part IV: investigation of the chromatographic efficiency dependent on the retention mode.

In our previous work we have described the synthesis, characterization, and optimization of the chromatographic efficiency of a highly crosslinked macroporous mixed-mode acrylamide-based monolithic stationary phase synthesized by in situ free radical copolymerization of cyclodextrin-solubilized N-adamantyl acrylamide, piperazinediacrylamide, methacrylamide and vinylsulfonic acid in aqueous medium in pre-treated fused silica capillaries of 100µm I.D. In the present work, we study with different classes of neutral analytes (with varied hydrophobicity) the impact of the type of retention mode (influenced by the type of analyte and the mobile phase composition) and the impact of the solute functionality on the chromatographic efficiency and peak symmetry with a monolith synthesized under optimized synthesis parameters. With this monolithic capillary high separation efficiencies (up to ca. 220,000m(-1)) are obtained for the separation of different analyte classes (alkylphenones, nitrotoluenes, and phenolic compounds with k=0.2-0.55) in the reversed-phase mode, in the normal-phase mode, and in the mixed mode. For neutral alkylanilines (k<0.25) plate numbers of about 300,000m(-1) are routinely reached in the reversed-phase elution mode. For phenolic solutes separated in a mixed mode there is a solute-specific influence on peak symmetry and chromatographic efficiency. With increasing efficiency of the monolith, axial diffusion becomes an important mechanism of band broadening. For those peaks, which do not show a significant asymmetry (asymmetry factor ≤1.05), it is confirmed that plate heights gained via the tangent method are equivalent to those gained via moment analysis.

Adamantyl-group containing mixed-mode acrylamide-based continuous beds for capillary electrochromatography. Part III. Optimization of the chromatographic efficiency.

In a previous article we described the synthesis of amphiphilic monolithic stationary phases by in situ free radical copolymerization of cyclodextrin-solubilized N-adamantyl acrylamide, piperazinediacrylamide, methacrylamide and vinylsulfonic acid in aqueous medium in pre-treated fused silica capillaries of 100µ.m I.D. In this work, a series of N-adamantyl-group containing acrylamide-based continuous beds is synthesized under variation of different synthesis parameters. The studied synthesis parameters are (i) concentration of the lyotropic salt ammonium sulfate, (ii) concentration of the initiator ammonium persulfate, and (iii) concentration of the negatively charged monomer vinylsulfonic acid in the polymerization mixture. The influence of the synthesis parameters on the chromatographic efficiency is studied under isocratic conditions for a homologues series of alkylphenones in the reversed-phase mode at constant composition of the mobile phase via capillary electrochromatography with varied electric field strength. With varied concentration of the lyotropic salt ammonium sulfate or varied concentration of the initiator ammonium persulfate in the polymerization mixture, a strong impact on the chromatographic efficiency is observed, while there is only a minor influence when varying the molar fraction of the charged monomer VSA. The absence of a significant influence of extra-column band broadening effects on the determined efficiency is confirmed. There is a good repeatability (with respect to capillary-to-capillary variation and run-to-run variation) reached for the theoretical plate heights obtained for DMF and selected alkylphenones in the reversed-phase mode.

Adamantyl-group containing mixed-mode acrylamide-based continuous beds for capillary electrochromatography. Part I: study of a synthesis procedure including solubilization of N-adamantyl-acrylamide via complex formation with a water-soluble cyclodextrin.

A new synthesis procedure for highly crosslinked macroporous amphiphilic N-adamantyl-functionalized mixed-mode acrylamide-based monolithic stationary phases for capillary electrochromatography (CEC) is investigated employing solubilization of the hydrophobic monomer by complexation with a cyclodextrin. N-(1-adamantyl)acrylamide is synthesized and characterized as a hydrophobic monomer forming a water soluble-inclusion complex with statistically methylated-ß-cyclodextrin. The stoichiometry, the complex formation constant and the spatial arrangement of the formed complex are determined. Mixed-mode monolithic stationary phases are synthesized by in situ free radical copolymerization of cyclodextrin-solubilized N-adamantyl acrylamide, a water soluble crosslinker (piperazinediacrylamide), a hydrophilic monomer (methacrylamide), and a negatively charged monomer (vinylsulfonic acid) in aqueous medium in bind silane-pretreated fused silica capillaries. The synthesized monolithic stationary phases are amphiphilic and can be employed in the reversed- and in the normal-phase mode (depending on the composition of the mobile phase), which is demonstrated with polar and non-polar analytes. Observations made with polar analytes and polar mobile phase can only be explained by a mixed-mode retention mechanism. The influence of the total monomer concentration (%T) on the chromatographic properties, the electroosmotic mobility, and on the specific permeability is investigated. With a homologues series of alkylphenones it is confirmed that the hydrophobicity (methylene selectivity) of the stationary phase increases with increasing mass fraction of N-(1-adamantyl)acrylamide in the synthesis mixture.