ABSTRACT
In this work a simple and novel procedure for leucomalachite green determination based on micro flow injection analysis (µFIA) with amperometric detection is presented. The method involves the use of henequen modified fibers as microfluidic channels. The µFIA system proposed offers a simple, rapid, and low-cost alternative for the determination. Capillary and gravitational forces across the modified henequen fibers control the flow rate, eliminating the need for external pumps. This technique requires low reagent consumption and allows portability for in situ measurements. The flow system is described, and the operational variables were studied and optimized using a Taguchi parameters design to increase analytical sensitivity. Under optimal conditions a limit of detection of 1.16 µg kg-1 was achieved with adequate repeatability and reproducibility (expressed as %RSD <5.0%, n = 3, n = 9 respectively) in all cases. The effect of interfering species and the accuracy of the method were also investigated. The proposed methodology was validated and applied to determine LMG in tilapia muscle samples.
ABSTRACT
In this work, a procedure using solid phase microextraction in combination with capillary electrophoresis was developed for the determination of oxytetracycline in milk samples. The method involves the synthesis of poly(1-allyl-3-methyl imidazolium) chloride film on a stainless-steel bar via electropolymerization and its use as an adsorbent for oxytetracycline (OT) by an ionic exchange mechanism. The coated fiber is then immersed in milk samples for retention of oxytetracycline residues, followed by elution, drying, and reconstitution before analysis with capillary electrophoresis. The proposed method achieves a limit of detection of 70 µg L⻹ with adequate precision and uncertainty, making this methodology appropriate for the determination of OT in milk samples. The method was applied to the pre-concentration and quantification of oxytetracycline in ten commercial milk samples. Two tested samples were positive for the presence of oxytetracycline but the concentration was below the maximum residue limit according to the international normative standard. The proposed methodology was evaluated according to the Eco-Scale approach, and the total score of 51 indicated that the methodology proposed is both green and acceptable despite the multi-stage character. SPME-CE methodology allows us to perform the sample pre-treatment and determination of OT in an effective and greener way, decreasing the number of steps during the analysis and the generation of waste.
Subject(s)
Ionic Liquids/chemistry , Milk/chemistry , Oxytetracycline/analysis , Polymers/chemistry , Allyl Compounds/chemistry , Animals , Dietary Fiber , Electrophoresis, Capillary , Imidazoles/chemistry , Polymerization , Solid Phase MicroextractionABSTRACT
In this work an electrochemical procedure for Cr(VI) flow based determination in tap water is presented. An AdCSV method was developed using a screen printed electrode modified with magnetic poly(1-allyl-3-methylimidazolium) chloride and the procedure does not require the addition of complexing agents in the solution unlike the methodologies reported so far for Cr(VI) determination. The flow based system is described and the control variables were studied in detail and optimized using a Taguchi parameters design. Under optimal conditions, the electrochemical sensor offered an excellent response to Cr(VI) and the limit of detection estimated from 3σ was 0.5⯵gâ¯L-1 (nâ¯=â¯3) allowing the analysis of tap water samples. The effect of interfering ions was also investigated below the maximum permissible limits for tap water according to Mexican standards. The presence of the magnetic particles on the sorbent allowed its easy modification on the electrode surface between each determination when removing the magnetic field placed in the wall-jet cell. Finally, the precision of the method was tested with tap water samples using standard addition method for Cr(VI) quantification and the accuracy was evaluated comparing the results with the dyphenylcarbazide method and by analyzing a certified water sample. The method shows good repeatability and reproducibility (%RSD less than 5%) making it feasible for Cr(VI) flow based determination and no significant difference is observed in the results obtained by both methods.