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An analytical method has been developed for the separation of glyoxal (Go), methylglyoxal (MGo), and dimethylglyoxal (DMGo) by MEKC using stilbenediamine (SD) as derivatizing reagent, separation time 6.5 min, SDS as micellar medium at pH 8, and sodium tetraborate (0.1 M) as buffer. Uncoated fused-silica capillary, effective length 50 cm x 75 microm id; applied voltage 20 kV and photodiode array detection, were used. Calibration was linear within 0.02-150 microg/mL with detection limits 3.5-5.8 ng/mL. Go and MGo, observed for diabetic and healthy volunteers, were within 0.098-0.193 microg/mL Go and 0.106-0.245 microg/mL MGo with RSD 1.6-3.5 and 1.7-3.4%, respectively, in diabetics against 0.016-0.046 microg/mL Go and 0.021-0.066 microg/mL MGo with RSDs 1.5-3.5 and 1.4-3.6%, respectively, in healthy volunteers. Go and MGo in diabetics were also measured by standard addition and DMGo as an internal standard. Additives do not contribute significantly to Go and MGo matrix.

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ABSTRACT:In water stressed Karachi city, waste water is often used for irrigating vegetables fields. Persistent use of waste water causes accumulation of heavy metals in agricultural soils and vegetables. Cd, Cr, Zn and Mn act as essential micronutrients but become toxic after crossing threshold values. To study the effect of waste water on heavy metal concentration in vegetables, soil and water an area irrigated separately with waste water and treated water were selected. Concentrations of Cd, Cr, Zn and Mn in beet, potato and radish were measured by atomic absorption spectrophotometer. The data obtained was tested at 95% (±2s) confidence level for six replicate measurements. The levels of Zn was found higher in both the treated water and vegetables beet, potato and radish irrigated with treated water but Mn was higher in industrial waste water and soil irrigated with industrial waste water and treated water. Soil irrigated with treated water contained (mg.

A micellar electrokinetic capillary chromatographic (MEKC) procedure has been developed for the separation and determination of dioxouranium (VI), iron(III), copper(II), and nickel(II) using bis(salicylaldehyde)propylenediimine (H2SA2Pn) as chelating reagent with a total run time of <3 min. Sodium dodecyl sulphate (SDS) was used as micellar medium at pH 8.1 with sodium tetraborate buffer (0.1 M). Uncoated fused silica capillary with effective length 38.8 cmx75 microm id was used with an applied voltage of 30 kV and photo-diode array detection at 228 nm. Linear calibrations were established within 0.045-1000 microg/mL of each element with detection limit within 15-122 ng/mL. The method was applied to the analysis of spring water and rock samples. The presence of uranium in rock and spring water samples was established within 1.58-1739.3 microg/g and 0.047-0.712 microg/mL with relative standard deviation within 0.9-2.1% and 1.3-2.6% respectively. Uranium ore and water samples were also assayed by the standard addition technique. Recovery of uranium was >98% with RSD up to 2.7%. Copper, nickel, and iron in their combined matrix were concurrently determined within RSD 0.6-3.6% (n=5) and the results obtained were compared with those of flame AAS.