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Abstract
OPTIMIZATION OF A MULTI-STEP EXTRACTION METHOD IN ANALYTICAL CHEMISTRY
Arshed Abdali Shihad*
ABSTRACT
The preparation of the sample is a very important procedure in the field of analytical chemistry especially where the analytes of interest are present in trace amounts in complex samples. In this paper, the optimization and development of a multi-step extraction process is introduced through a systematic and statistically justified process. The adaptation of a fractional factorial design was initially used to filter out important extraction parameters, and response surface methodology was then used to determine the most desirable conditions and determine the effects of interactions. The optimised procedure employed acetonitrile as the extraction solvent, 18 mL as the volume of solvent and 6.2 to indicate the pH of the sample, which made the average analyte recovery to be 93.8 + 1.5 percent with the relative standard deviations less than 3 percent. The validation of the method showed that it had a high linearity (R 2 = 0.998), low limits of detection and quantification (0.12 ugkg -1 and 0.40 ugkg -1, respectively), and a high degree of accuracy, over the various concentrations of the experiment. The streamlined protocol did not only improve the efficiency and reproducibility of extraction, but also reduced the use of solvent and the workload of the experiment. The results obtained indicated the usefulness of multivariate optimization schemes in enhancing multi-step extraction procedures, which is a sound and viable mechanism of analyzing traces in intricate matrices.
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