title: Optimization of dispersive liquid-phase microextraction based on solidified floating organic drop combined with high-performance liquid chromatography for the analysis of glucocorticoid residues in food.
abstract: A rapid, simple, cost-effective dispersive liquid-phase microextraction based on solidified floating organic drop (SFOD-LPME) was developed in this study. Along with high-performance liquid chromatography, we used the developed approach to determine and enrich trace amounts of four glucocorticoids, namely, prednisone, betamethasone, dexamethasone, and cortisone acetate, in animal-derived food. We also investigated and optimized several important parameters that influenced the extraction efficiency of SFOD-LPME. These parameters include the extractant species, volumes of extraction and dispersant solvents, sodium chloride addition, sample pH, extraction time and temperature, and stirring rate. Under optimum experimental conditions, the calibration graph exhibited linearity over the range of 1.2-200.0ng/ml for the four analytes, with a reasonable linearity(r2: 0.9990-0.9999). The enrichment factor was 142-276, and the detection limits was 0.39-0.46ng/ml (0.078-0.23μg/kg). This method was successfully applied to analyze actual food samples, and good spiked recoveries of over 81.5%-114.3% were obtained.
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China.
authors.forename: Yuan
authors.initials: Y
authors.lastname: Huang
authors.affiliation: Union Affiliated to Fujian Medical University, Fuzhou Fujian 350003, China.
authors.forename: Zhiqun
authors.initials: Z
authors.lastname: Zheng
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China. Electronic address: fjmuhly88@sina.com.cn.
authors.forename: Liying
authors.initials: L
authors.lastname: Huang
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China.
authors.forename: Hong
authors.initials: H
authors.lastname: Yao
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China; Department of Pharmacy, Fujian Health College, Fuzhou, 350101, China.
authors.forename: Xiao Shan
authors.initials: XS
authors.lastname: Wu
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China.
authors.forename: Shaoguang
authors.initials: S
authors.lastname: Li
authors.affiliation: College of Pharmacy, Fujian Medical University, Fuzhou Fujian 350108, China.
authors.forename: Dandan
authors.initials: D
authors.lastname: Lin
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005502:Food; D005504:Food Analysis / Q000379:methods*; D005938:Glucocorticoids / Q000737:chemistry*; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry; D013696:Temperature
chemical_list: D005938:Glucocorticoids; D012997:Solvents
keywords: Animal-derived food; Determination and enrichment; Glucocorticoid residues; High-performance liquid chromatography; Liquid-phase microextraction based on solidification of floating organic drop