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1.
Mikrochim Acta ; 190(12): 464, 2023 11 10.
Artículo en Inglés | MEDLINE | ID: mdl-37947885

RESUMEN

A novel and efficient on-line microextraction on a screw coupled with high-performance liquid chromatography with an ultraviolet-visible detector was developed to extract and determine trace quantities of five opium alkaloids. All detections of the analytes were achieved at 210 nm. The surface of the screw grooves was electrochemically coated with the carbon nanotubes-COOH/polyaniline composite. The surface characterization was assessed by Fourier transform infrared spectroscopy and field emission scanning electron microscopy. The prepared screw was inserted into a cartridge of a guard column, and then the constructed microextraction on a screw device was placed in the loop of a six-port HPLC injection valve. The parameters affecting the extraction efficiency of the analytes were optimized using the one variable-at-a-time method. The effective parameters for the extraction efficiency of the analytes, including sample volume, extraction time, sampling flow rate, desorption solvent type, ionic strength, and pH were investigated and optimized. Under optimal conditions, the detection limits were 3-10 µg L-1, and the linear dynamic ranges were 10-2000 µg L-1 with a coefficient of determination greater than 0.9940. The inter-day and intra-day (n = 3) relative standard deviations were less than 7% and 5%, respectively. The proposed method was simple and reproducible, with an acceptable relative recovery (90-108%) for determining opium alkaloids in water and urine samples.


Asunto(s)
Alcaloides , Nanotubos de Carbono , Cromatografía Líquida de Alta Presión/métodos , Nanotubos de Carbono/química , Opio , Límite de Detección
2.
J Sep Sci ; 46(22): e2300421, 2023 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-37688348

RESUMEN

In the present work, a novel solid-phase microextraction on a screw (MES) was employed to extract cationic dyes (malachite green, methylene blue, and rhodamine B) from food samples and fish breeding pool water. The sulfonated poly(styrene-co-divinylbenzene) was electrophoretically deposited on the surface of the grooves of a screw. Then the screw was placed inside a silicon tube as a holder to create a channel to run a test solution through it. The extracted dyes on the coated screw were eluted by a suitable eluent. High-performance liquid chromatography with an ultraviolet/visible detector was utilized for the separation and analysis of the analytes. The effective parameters of the analyte extraction efficiency were optimized. Under optimum conditions, the limits of detection were 0.15 µg/L, and calibration curves were linear in the range of 0.50-250.00 µg/L, with coefficients of determination > 0.989 for all studied dyes. The relative standard deviations of intra and inter-day (n = 3) were in the range of 2.8%-7.0% and 7.0%-9.5%, respectively. The MES was applied as a simple and repeatable method with acceptable relative recoveries (82.0%-103.0%) for the determination of cationic dyes in grape nectar, ice pop, jelly powder, and fish breeding pool water.

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