Novel capsule phase microextraction in combination with high performance liquid chromatography with diode array detection for rapid monitoring of sulfonamide drugs in milk.

Capsule phase microextraction is introduced herein for the first time to determine four sulfonamide residues in milk samples (sulfanilamide, sulfadiazine, sulfamethizole, and sulfathiazole). The technique eloquently integrates filtration and stirring mechanism into the extraction device, as such no filtration of the sample is needed prior to introducing the extraction device into the sample, and when placed on a magnetic stirrer, the device spins itself in order to diffuse the sample, resulting in faster extraction equilibrium. Microextraction capsules consist of three main parts; a magnet, a cellulose fiber substrate coated with high performance sol-gel hybrid organic-inorganic sorbent, and a porous membrane. Various encapsulated sol-gel sorbents were tested in standard solutions prepared in deionized water and milk samples under different operational conditions. Analyte extraction time and elution time, type of sol-gel sorbent, elution solvent, as well as the ratio of the sorbent to the elution solvent were among the optimized conditions. The protocols that yielded the best absolute recovery rates were subsequently tested in various milk samples. Method validation was performed in terms of linearity, accuracy and precision, reusability and ruggedness using the Youden test. The examined sulfonamides were subsequently analysed by reversed phase high performance liquid chromatography with diode array detection.

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