Toxin Research Center, AJA University of Medical Sciences, Tehran, Iran.
Toxin Research Center, AJA University of Medical Sciences, Tehran, Iran.
Talanta. 2018 May 15;182:299-305. doi: 10.1016/j.talanta.2018.02.002. Epub 2018 Feb 2.
A novel and efficient device of solvent stir-bar microextraction (SSBME) system coupled with GC-FID detection was introduced for the pre-concentration and determination of malondialdehyde (MDA) in different biological matrices. In the proposed device, a piece of porous hollow fiber was located on a magnetic rotor by using a stainless steel-wire (as a mechanical support) and the whole device could stir with the magnetic rotor in sample solution cell. The device provided higher pre-concentration factor and better precision in comparison with conventional SBME due to the reproducible, stable and high contact area between the stirred sample and the hollow fiber. Organic solvent type, donor and acceptor phase pH, temperature, electrolyte concentration, agitation speed, extraction time, and sample volume as the effective factors on the SSBME efficiency, were examined and optimized. Pure tris-(2-ethylhexyl) phosphate (TEHP) was examined for the first time as supported liquid membrane (SLM) for the determination of MDA by SSBME method. In contrast to the conventional SLMs of SBME in the literature, the SLM of TEHP was highly stable in contact with biological fluids and provided the highest extraction efficiency. Under optimized extraction conditions, the method provided satisfactory linearity in the range 1-500 ng mL, low LODs (0.3-0.7 ng mL), good repeatability and reproducibility (RSD% (n = 5) < 4.5) with the pre-concentration factors higher than 130-fold. To verify the accuracy of the proposed method, the traditional spectrophotometric TBA (2-thiobarbituric acid) test was used as a reference method. Finally, the proposed method was successfully applied for the determination and quantification of MDA in biological fluids.
一种新颖高效的溶剂搅拌棒微萃取(SSBME)系统与 GC-FID 检测相结合,用于不同生物基质中丙二醛(MDA)的预浓缩和测定。在所提出的装置中,通过使用不锈钢丝(作为机械支撑)将一块多孔中空纤维置于磁性转子上,整个装置可以与磁性转子在样品溶液池中一起搅拌。与传统的 SBME 相比,该装置由于搅拌样品与中空纤维之间具有可重复、稳定和高的接触面积,因此提供了更高的预浓缩因子和更好的精密度。考察并优化了有机溶剂类型、供体和受体相 pH 值、温度、电解质浓度、搅拌速度、萃取时间和样品体积等因素对 SSBME 效率的影响。首次考察了纯三(2-乙基己基)磷酸酯(TEHP)作为支持液膜(SLM)用于 SSBME 法测定 MDA。与文献中 SBME 的传统 SLM 相比,TEHP 的 SLM 在与生物流体接触时高度稳定,提供了最高的萃取效率。在优化的萃取条件下,该方法在 1-500ng/mL 的范围内提供了令人满意的线性关系,低检测限(0.3-0.7ng/mL),良好的重复性和重现性(RSD%(n=5)<4.5),预浓缩因子高于 130 倍。为了验证该方法的准确性,采用传统的分光光度法 TBA(2-硫代巴比妥酸)试验作为参考方法。最后,该方法成功应用于生物流体中 MDA 的测定和定量。