A novel micro-extraction strategy for extraction of bisphosphonates from biological fluids using zirconia nanoparticles coupled with spectrofluorimetry and high performance liquid chromatography

• Published in: Yàowu shi͡p︡in fenxi 2018-10, Vol.26 (4), p.1303-1311
• Main Authors: Rahbar, Nadereh, Nazernezhad, Ladan, Asadinezhad, Maryam, Ramezani, Zahra, Kouchak, Maryam
• Format: Article
• Language: English
• Subjects: 2-Mercaptoethanol; Adsorption; Alendronate - blood; Alendronate - isolation & purification; Alendronate - urine; Alendronate sodium; Alendronic acid; Bisphosphonates; Chemisorption; Chromatography; Chromatography, High Pressure Liquid - methods; Dispersive micro solid phase extraction; Fluorescence; High performance liquid chromatography; Humans; Limit of Detection; Liquid chromatography; Measurement methods; Measuring methods; Methods; Nanoparticles; Nanoparticles - chemistry; O-phthalaldehyde; Organic chemistry; Original; Sample preparation; Serum - chemistry; Sodium; Solid Phase Microextraction - instrumentation; Solid Phase Microextraction - methods; Solid phases; Spectrofluorimetry; Spectrometry, Fluorescence - methods; Urine; Urine - chemistry; Zirconia; Zirconia nanoparticles; Zirconium - chemistry; Zirconium dioxide; ZrO2
• ISSN: 1021-9498; 2224-6614
• DOI: 10.1016/j.jfda.2018.03.005

Extraction of bisphosphonates from biological fluids is important and time consuming step in sample preparation procedure. This paper describes a simple and green sample preparation technique for dispersive micro solid phase extraction (DMSPE) of alendronate sodium (ALS) from urine and serum samples prior to direct spectrofluorimetry (DSFL) and high performance liquid chromatography with fluorescence detection (HPLC-FLD), respectively. The DMSPE strategy is based on the selective chemisorption of ALS on zirconia nanoparticles (ZNPs) as an adsorbent followed by derivatization of the eluted analyte using o-phthalaldehyde (OPA) in the presence of 2-mercaptoethanol (2ME) at basic medium to form fluorescent species. The chemical and instrumental influencing parameters on DMSPE and measuring methods were optimized for the efficient extraction and determination of ALS. The presented methods were capable of extracting ALS from human urine and serum samples and determining over the wide ranges of 5–1000 and 5–2500 μg L−1 with limits of detection (LOD) of 1.5 and 1.4 μg L−1 for DSFL and HPLC methods, respectively. The relative recoveries for the three spiked standard levels of ALS in urine and serum samples ranged from 89.0% to 107.0%, and the intra-day relative standard deviations (%RSDs) were in the range of 2.9–7.9%. [Display omitted] •We have introduced a new method for extraction of ALS by applying ZNPs. This is the first time ZNP was applied as solid phase for extraction of bisphosphonates from biological matrices.•In this work application of direct spectrofluorimetric detection of ALS after derivatization in biological fluids is reported for first time.•Selective extraction of ALS by ZNP allows the development of simple, low cost, rapid and safe operation in comparison to laborious conventional precipitation method.•Combination of MSPE using ZNP with spectrofluorimetric and HPLC-FLD detection techniques has merits of selectivity and sensitivity for analysis of ALS in biological fluids.•The proposed procedure was successfully applied for determination of ALS at low concentrations in human serum and urine samples.