Combination of magnetic dispersive micro solid-phase extraction and supramolecular solvent-based microextraction followed by high-performance liquid chromatography for determination of trace amounts of cholesterol-lowering drugs in complicated matrices

• Published in: Analytical and bioanalytical chemistry Vol. 409; no. 18; pp. 4395 - 4407
• Main Authors: Arghavani-Beydokhti, Somayeh, Rajabi, Maryam, Asghari, Alireza
• Format: Journal Article
• Language: English
• Published: Berlin/Heidelberg Springer Berlin Heidelberg 01-07-2017; Springer; Springer Nature B.V
• Subjects: Analytical Chemistry; Anticholesteremic agents; Atorvastatin; Biochemistry; Centrifugation; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Cholesterol; Chromatography; Chromatography, High Pressure Liquid; Deionization; Dispersion; Elution; Emulsification; Extraction (Chemistry); Extraction processes; Food Science; Gemfibrozil; High performance liquid chromatography; Hydrogen-Ion Concentration; Hydroxides; Hydroxymethylglutaryl-CoA Reductase Inhibitors - chemistry; Iron oxides; Laboratory Medicine; Linearity; Liquid chromatography; Liquid Phase Microextraction - methods; Magnetics; Methods; Microscopy, Acoustic; Monitoring/Environmental Analysis; Nanoparticles; Research Paper; Solid Phase Extraction - methods; Solvents; Testing; Ultraviolet radiation; Magnetic dispersive micro solid-phase extraction; Complicated matrices; Layered double hydroxide-coated magnetic nanoparticles; Supramolecular solvent-based microextraction
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-017-0383-x

A novel, efficient, rapid, simple, sensitive, selective, and environmentally friendly method termed magnetic dispersive micro solid-phase extraction combined with supramolecular solvent-based microextraction (Mdμ-SPE–SSME) followed by high-performance liquid chromatography (HPLC) with UV detection is introduced for the simultaneous microextraction of cholesterol-lowering drugs in complicated matrices. In the first microextraction procedure, using layered double hydroxide (LDH)-coated Fe
3
O
4
magnetic nanoparticles, an efficient sample cleanup is simply and rapidly provided without the need for time-consuming centrifugation and elution steps. In the first step, desorption of the target analytes is easily performed through dissolution of the LDH-coated magnetic nanoparticles containing the target analytes in an acidic solution. In the next step, an emulsification microextraction method based on a supramolecular solvent is used for excellent preconcentration, ultimately resulting in an appropriate determination of the target analytes in real samples. Under the optimal experimental conditions, the Mdμ-SPE–SSME–HPLC–UV detection procedure provides good linearity in the ranges of 1.0–1500 ng mL
-1
, 1.5–2000 ng mL
-1
, and 2.0–2000 ng mL
-1
with coefficients of determination of 0.995 or less, low limits of detection (0.3, 0.5, and 0.5 ng mL
-1
), and good extraction repeatabilities (relative standard deviations below 7.8%,
n
= 5) in deionized water for rosuvastatin, atorvastatin, and gemfibrozil, respectively. Finally, the proposed method is successfully applied for the determination of the target analytes in complicated matrices.
Graphical Abstract
Mdμ-SPE–SSME procedure