Sadeghi Sahar, Mollahosseini Afsaneh
Research Laboratory of Spectroscopy & Micro and Nano Extraction, Department of Chemistry, Iran University of Science and Technology, Tehran, Iran.
Research Laboratory of Spectroscopy & Micro and Nano Extraction, Department of Chemistry, Iran University of Science and Technology, Tehran, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jan 15;1073:43-50. doi: 10.1016/j.jchromb.2017.11.042. Epub 2017 Dec 10.
In this study, polydimethylsiloxane/polyacrylonitrile/titanium dioxide (PDMS/PAN/TiO) nanofibers were synthesized via electrospinning method to extract and quantify alpha-linolenic acid (ALA, C18:3), as a model analyte, in milk by direct immersion-solid phase nanoextraction (DI-SPNE) with gas chromatography-flame ionization detector (GC-FID). The affecting factors on the electrospinning process such as, PDMS concentration, amount of TiO nanoparticles (NPs), voltage, and electrospinning distance were optimized using Taguchi's orthogonal design. The SPNE experimental conditions such as, extraction time, agitation rate, pH and salt concentration, were also optimized using response surface methodology (RSM) based on a central composite design (CCD). Under optimized conditions, the resulting calibration curve was linear in the range of 1-4000ngmL with R=0.998. The intraday, interday, and fiber-to-fiber repeatability were calculated and the corresponding relative standard deviation was less than 9% in all the cases. The limit of detection and limit of quantification were found to be 0.2 and 0.6ngmL, respectively. Omega-3 enriched milk was used as a real sample and the value of relative recoveries were measured to be in the range of 92-106%.
在本研究中,通过静电纺丝法合成了聚二甲基硅氧烷/聚丙烯腈/二氧化钛(PDMS/PAN/TiO)纳米纤维,以通过气相色谱 - 火焰离子化检测器(GC - FID)的直接浸入 - 固相纳米萃取(DI - SPNE)来提取和定量牛奶中的α - 亚麻酸(ALA,C18:3)作为模型分析物。使用田口正交设计优化了静电纺丝过程中的影响因素,如PDMS浓度、TiO纳米颗粒(NPs)的量、电压和静电纺丝距离。还基于中心复合设计(CCD)使用响应面方法(RSM)优化了SPNE实验条件,如萃取时间、搅拌速率、pH值和盐浓度。在优化条件下,所得校准曲线在1 - 4000ng/mL范围内呈线性,R = 0.998。计算了日内、日间和纤维间的重复性,在所有情况下相应的相对标准偏差均小于9%。检测限和定量限分别为0.2和0.6ng/mL。使用富含ω-3的牛奶作为实际样品,测得相对回收率的值在92 - 106%范围内。