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A novel micro-extraction strategy for extraction of bisphosphonates from biological fluids using zirconia nanoparticles coupled with spectrofluorimetry and high performance liquid chromatography
Journal of Food and Drug Analysis ( IF 3.6 ) Pub Date : 2018-10-01 , DOI: 10.1016/j.jfda.2018.03.005
Nadereh Rahbar 1, 2 , Ladan Nazernezhad 2 , Maryam Asadinezhad 3 , Zahra Ramezani 1, 2 , Maryam Kouchak 1, 4
Affiliation  

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%.

中文翻译:

一种使用氧化锆纳米粒子结合荧光分光光度法和高效液相色谱法从生物体液中提取双膦酸盐的新型微萃取策略

从生物体液中提取双膦酸盐是样品制备过程中重要且耗时的步骤。本文介绍了一种简单且绿色的样品制备技术,用于在直接分光荧光法 (DSFL) 和带荧光检测的高效液相色谱法 (HPLC-FLD) 之前从尿液和血清样品中进行阿仑膦酸钠 (ALS) 的分散微固相萃取 (DMSPE) , 分别。DMSPE 策略基于 ALS 在作为吸附剂的氧化锆纳米粒子 (ZNP) 上的选择性化学吸附,然后在碱性介质中的 2-巯基乙醇 (2ME) 存在下使用邻苯二甲醛 (OPA) 衍生洗脱的分析物以形成荧光物种。优化了对 DMSPE 的化学和仪器影响参数和测量方法,以实现 ALS 的高效提取和测定。所提出的方法能够从人类尿液和血清样品中提取 ALS,并在 5-1000 和 5-2500 μg L-1 的宽范围内测定 DSFL 和 1.5 和 1.4 μg L-1 的检测限 (LOD) 和HPLC方法,分别。尿液和血清样品中 ALS 的三种加标标准水平的相对回收率范围为 89.0% 至 107.0%,日内相对标准偏差 (%RSD) 范围为 2.9-7.9%。分别。尿液和血清样品中 ALS 的三种加标标准水平的相对回收率范围为 89.0% 至 107.0%,日内相对标准偏差 (%RSD) 范围为 2.9-7.9%。分别。尿液和血清样品中 ALS 的三种加标标准水平的相对回收率范围为 89.0% 至 107.0%,日内相对标准偏差 (%RSD) 范围为 2.9-7.9%。
更新日期:2018-10-01
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