Parham Hooshang, Rahbar Nadereh
Department of Chemistry, Shahid Chamran University, Ahvaz, Iran.
J Pharm Biomed Anal. 2009 Aug 15;50(1):58-63. doi: 10.1016/j.jpba.2009.03.037. Epub 2009 Apr 7.
This method shows a novel, fast and simple solid phase extraction-spectrophotometric procedure for preconcentration and determination of salicylic acid (SA) in blood serum using magnetic iron oxide nanoparticles (MIONs) as extractor. It is shown that the novel magnetic nano-adsorbent is quite efficient for fast adsorption of SA at 25 degrees C. Various parameters affecting the adsorption of SA on MIONs, such as pH of solution, type, volume and concentration of desorbing reagent and amount of adsorbent and matrix effects, have been investigated. The calibration graph for the determination of SA was linear in the range of 0.025-1.250microgmL(-1). The limit of detection (LOD) based on three times the standard deviation of the blank (3S(b)) was 5.5x10(-3)microgmL(-1) (n=10) for SA. The intra-day precision (R.S.D.) was below 10.1% and inter-day R.S.D. was less than 17.5%, while accuracy (relative error R.E.) was within +/-3.6 determined from quality control samples for salicylic acid (SA) which corresponded to requirement of the guidance of Food and Drug Administration (FDA). The preconcentration factor of 100 was achieved in this method. The proposed procedure has been successfully applied to the determination of SA in blood serum.
该方法展示了一种新颖、快速且简单的固相萃取-分光光度法,用于以磁性氧化铁纳米颗粒(MIONs)作为萃取剂对血清中的水杨酸(SA)进行预富集和测定。结果表明,这种新型磁性纳米吸附剂在25℃下对SA具有高效快速的吸附能力。研究了影响SA在MIONs上吸附的各种参数,如溶液pH值、解吸剂的类型、体积和浓度、吸附剂用量以及基质效应等。测定SA的校准曲线在0.025 - 1.250μg/mL范围内呈线性。基于空白标准偏差的三倍(3S(b)),SA的检测限(LOD)为5.5×10⁻³μg/mL(n = 10)。日内精密度(相对标准偏差,R.S.D.)低于10.1%,日间R.S.D.小于17.5%,而准确度(相对误差,R.E.)在±3.6范围内,这是根据对应于食品药品监督管理局(FDA)指南要求的水杨酸(SA)质量控制样品确定的。该方法实现了100倍的预富集因子。所提出的方法已成功应用于血清中SA的测定。