Roosta Mostafa, Ghaedi Mehrorang, Daneshfar Ali, Sahraei Reza
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
J Chromatogr B Analyt Technol Biomed Life Sci. 2015 Jan 15;975:34-9. doi: 10.1016/j.jchromb.2014.10.035. Epub 2014 Nov 3.
In the present study, for the first time, a new extraction method based on "ultrasound assisted microextraction-nanomaterial solid phase dispersion (UAME-NMSPD)" was developed to preconcentrate the low quantity of thymol and carvacrol in pharmaceutical samples prior to their HPLC-UV separation/determination. The analytes were accumulated on nickel sulfide nanomaterial loaded on activated carbon (NiS-NP-AC) that with more detail identified by XRD, FESEM and UV-vis technique. Central composite design (CCD) combined with desirability function (DF) was used to search for optimum operational conditions. Working under optimum conditions specified as: 10 min ultrasonic time, pH 3, 0.011 g of adsorbent and 600 μL extraction solvent) permit achievement of high and reasonable linear range over 0.005-2.0 μg mL(-1) (r(2)>0.9993) with LOD of thymol and carvacrol as 0.23 and 0.21 μg L(-1), respectively. The relative standard deviations (RSDs) were less than 4.93% (n=3).
在本研究中，首次开发了一种基于“超声辅助微萃取-纳米材料固相分散（UAME-NMSPD）”的新萃取方法，用于在高效液相色谱-紫外（HPLC-UV）分离/测定之前对药物样品中低含量的百里香酚和香芹酚进行预富集。分析物富集在负载于活性炭上的硫化镍纳米材料（NiS-NP-AC）上，并用X射线衍射（XRD）、场发射扫描电子显微镜（FESEM）和紫外可见（UV-vis）技术进行了更详细的鉴定。采用中心复合设计（CCD）结合期望函数（DF）来寻找最佳操作条件。在指定的最佳条件下工作（超声时间10分钟、pH值3、吸附剂0.011克和萃取溶剂600微升），可实现0.005-2.0微克/毫升（-1）范围内高且合理的线性范围（r（2）>0.9993），百里香酚和香芹酚的检测限分别为0.23和0.21微克/升（-1）。相对标准偏差（RSD）小于4.93%（n = 3）。
