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

Abstract

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 FeO 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, 1.5-2000 ng mL, and 2.0-2000 ng mL with coefficients of determination of 0.995 or less, low limits of detection (0.3, 0.5, and 0.5 ng mL), 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.

A review on liquid chromatographic methods for the bioanalysis of atorvastatin

“…Most of the references cited in Tables 1 and 2 also describe the simultaneous determination of AT with certain other statins [13, 20, 24, 27-29, 50, 51, 54, 56, 61, 65, 81, 87] and other co-administered drugs such as amlodipine [35,40,59,64,65,69,70,77,78,95], ezetimibe [42,66,71], gemfibrozil [13,30,51], clopidogrel [14,15,41,93], fenofibrate [26], aspirin [15,23,72], ramipril [64,78], pioglitazone [17,22], glimepiride [64,68,73], olmesartan [62,98], and many other. Various methods have also been developed and validated using LC-MS/MS to quantify the metabolites of AT and are enlisted in Table 2 [54, 56-58, 60-62, 65, 67, 69, 70, 74-76, 79, 80, 82, 83, 85-91, 96, 100].…”

“…Identically, AlKhani et al designed a precise HPLC-UV method to quantify AT in both rat plasma and rat intestinal perfusion solution for its further application in pharmacokinetic studies [39]. The development of analytical methods for the detection of drugs and its metabolites in the urine samples generally helps to understand in vivo metabolism and clearance process, so, various methods have been developed to analyze AT in the urine samples [13,43,44,47,92]. In the year 2017, Beydokhti et al proposed a method to simultaneously determine AT, rosuvastatin, and gemfibrozil in deionized water, wastewater, human plasma, and urine using HPLC-UV method and urine samples were prepared for analysis by diluting with 10 mL of deionized water [13].…”

“…The development of analytical methods for the detection of drugs and its metabolites in the urine samples generally helps to understand in vivo metabolism and clearance process, so, various methods have been developed to analyze AT in the urine samples [13,43,44,47,92]. In the year 2017, Beydokhti et al proposed a method to simultaneously determine AT, rosuvastatin, and gemfibrozil in deionized water, wastewater, human plasma, and urine using HPLC-UV method and urine samples were prepared for analysis by diluting with 10 mL of deionized water [13]. Likewise, eight statins were simultaneous determined in human urine using a highly selective and sensitive LC-MS/MS method developed by Jang et al in which dilute and shot approach was used for urine sample preparation [92].…”

“…In the same way, Beydokhti et al developed a novel extraction technique by the combining magnetic dispersive micro SPE process and supra-molecular solvent-based microextraction process (Mdμ-SPE-SSME) to extract AT, rosuvastatin, and gemfibrozil from human plasma and urine sample with the help of layered double hydroxide-coated Fe 3 O 4 . Also, in comparison with the conventional SPE technique, Mdμ-SPE-SSME reduces the overall extraction time and eliminates the elution step [13]. Interestingly, Vlčková et al developed microextraction by packed sorbent (MEPS) technique to extract AT and its metabolites from biological samples using a gas-tight syringe as an extraction device [56,74].…”

Dissolvable layered double hydroxide nanoadsorbent‐based dispersive solid‐phase extraction for highly efficient and eco‐friendly simultaneous microextraction of two toxic metal cations and two anionic azo dyes in real samples

“…In this method, the adsorbent is directly added to the sample solution containing the target analytes, and the dispersion process is assisted by an external energy source such as vortex, air or sonication. Another important feature of the D‐SPE method is the variety of solid sorbents to achieve a specific selectivity and high extraction efficiency …”