Integration of phase separation with ultrasound-assisted salt-induced liquid–liquid microextraction for analyzing the fluoroquinones in human body fluids by liquid chromatography

Abstract

a b s t r a c tHerein, we developed a novel integrated device to perform phase separation based on ultrasound-assisted salt-induced liquid-liquid microextraction for determination of five fluoroquinones (FQs) in human body fluids. The integrated device consisted of three simple HDPE components used to separate the extraction solvent from the aqueous phase prior to retrieving the extractant. A series of extraction parameters were optimized using the response surface method based on central composite design. Optimal conditions consisted of 945 L acetone extraction solvent, pH 2.1, 4.1 min stir time, 5.9 g Na 2 SO 4 , and 4.0 min centrifugation. Under optimized conditions, the limits of detection (at S/N = 3) were 0.12-0.66 g L −1 , the linear range was 0.5-500 g L −1 and recoveries were 92.6-110.9% for the five FQs extracted from plasma and urine. The proposed method has several advantages, such as easy construction from inexpensive materials, high extraction efficiency, short extraction time, and compatibility with HPLC analysis. Thus, this method shows excellent prospects for sample pretreatment and analysis of FQs in human body fluids.© 2015 Elsevier B.V. All rights reserved.Abbreviations: PS-USLM, phase separation based on ultrasound-assisted, salt-induced, liquid-liquid microextraction; FQs, fluoroquinones; HPLC-FLD, high performance liquid chromatography equipped with fluorescence detector; PPCPs, pharmaceuticals and personal care products; HPLC, high performance liquid chromatography; MS, mass spectrometry; SPE, solid-phase extraction; LLE, liquid-liquid extraction; LPME, liquid-phase microextraction; DLLME, dispersive liquid-liquid microextraction; SALLME, salting-out assisted liquid-liquid microextraction; RSM, response surface method; CCD, central composite design; LOD, limits of detection; ER, extraction recovery; FLE, fleroxacin; OFL, ofloxacin; NOR, norfloxacin; CIP, ciprofloxacin; ENR, enrofloxacin; MgSO4, magnesium sulfate; Na2SO4, sodium sulfate; CH3COONa, sodium acetate; (NH4)2SO4, ammonium sulfate; CH3COONH4, ammonium acetate; HDPE, high-density polyethylene; LDR, linear dynamic range; RSDs, relative standard deviations; RR, relative recovery; LLE-HPLC, liquid-liquid extraction combined with high performance liquid chromatography; SPE-HPLC, solid phase extraction combined with high performance liquid chromatography; SOMC-HPLC, second-order multivariate calibration combined with high performance liquid chromatography; SSPC-HPLC, single-step precipitation cleanup method combined with high performance liquid chromatography; UFLC, ultra-fast liquid chromatography; HF-LPME-HPLC, hollow fiber-based liquid phase microextraction combined with high performance liquid chromatography.

Salt-Induced Liquid–Liquid Phase Separation: Combined Experimental and Theoretical Investigation of Water–Acetonitrile–Salt Mixtures

“…This phenomenon forms the basis for a widely used method called salting-out assisted liquid–liquid extraction (SALLE) − for the extraction and separation of chemicals. For example, the method has been used to extract pesticide residues from food − and environmental water, , drugs from animal blood and urine, − and active ingredients from herbal medicine . This method was discovered by Matkovich and Christian, who demonstrated the separation of acetone from aqueous solution on addition of salt .…”

“…Water–acetonitrile mixture is one of the most widely used systems in the applications of SALLE. − As such, it serves as an excellent model system for understanding the effects of salts on the phase behavior of the mixture. However, the fundamental physical chemistry on this topic, especially on the specific ion effects on the phase behaviors, has not been well studied.…”

A Green and Efficient Method for the Preconcentration and Determination of Gallic Acid, Bergenin, Quercitrin, and Embelin from Ardisia japonica Using Nononic Surfactant Genapol X-080 as the Extraction Solvent

“…The concentration of sodium dihydrogen phosphate is also a key factor in CPE [ 27 ]. The addition of salt to the sample solution can influence the extraction resulting from a changing in density of the aqueous phase [ 28 ]. The influence of the ionic strength on the extraction efficiency was carried out by changing the concentration of sodium dihydrogen phosphate between 15% and 35% (w/v).…”

Effective extraction and determination of 24 quinolones in water and egg samples using a novel magnetic covalent organic framework combined with UPLC-MS/MS

“…Nevertheless, the complicated matrix and extremely low concentration of QNs in food and water samples can influence detection results; therefore, an effective sample pretreatment is indispensable. Common sample pretreatment methods include liquid–liquid extraction(LLE), 13 dispersive liquid–liquid micro-extraction (DLLME), 14 solid phase extraction (SPE), 15–17 dispersive solid-phase extraction (DSPE) 18,19 and magnetic solid phase extraction (MSPE). 20–22 Different from conventional sample pretreatment methods, MSPE is a dispersed solid-phase extraction technique that uses magnetic materials as adsorbents to achieve the separation and enrichment of analytes by an external magnetic field.…”