Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Ultrason Sonochem. 2017 Sep;38:463-472. doi: 10.1016/j.ultsonch.2017.03.045. Epub 2017 Mar 28.
A sensitive analytical method is investigated to concentrate and determine trace level of Sildenafil Citrate (SLC) present in water and urine samples. The method is based on a sample treatment using dispersive solid-phase micro-extraction (DSPME) with laboratory-made Mn@ CuS/ZnS nanocomposite loaded on activated carbon (Mn@ CuS/ZnS-NCs-AC) as a sorbent for the target analyte. The efficiency was enhanced by ultrasound-assisted (UA) with dispersive nanocomposite solid-phase micro-extraction (UA-DNSPME). Four significant variables affecting SLC recovery like; pH, eluent volume, sonication time and adsorbent mass were selected by the Plackett-Burman design (PBD) experiments. These selected factors were optimized by the central composite design (CCD) to maximize extraction of SLC. The results exhibited that the optimum conditions for maximizing extraction of SLC were 6.0 pH, 300μL eluent (acetonitrile) volume, 10mg of adsorbent and 6min sonication time. Under optimized conditions, virtuous linearity of SLC was ranged from 30 to 4000ngmL with R of 0.99. The limit of detection (LOD) was 2.50ngmL and the recoveries at two spiked levels were ranged from 97.37 to 103.21% with the relative standard deviation (RSD) less than 4.50% (n=15). The enhancement factor (EF) was 81.91. The results show that the combination UAE with DNSPME is a suitable method for the determination of SLC in water and urine samples.
研究了一种灵敏的分析方法，用于浓缩和测定水样和尿样中痕量的西地那非（SLC）。该方法基于使用分散固相微萃取（DSPME）进行样品处理，以实验室制备的负载在活性炭上的 Mn@CuS/ZnS 纳米复合材料（Mn@CuS/ZnS-NCs-AC）作为目标分析物的吸附剂。通过超声辅助（UA）与分散纳米复合材料固相微萃取（UA-DNSPME）来增强效率。通过 Plackett-Burman 设计（PBD）实验选择了四个影响 SLC 回收率的显著变量，如 pH 值、洗脱体积、超声时间和吸附剂质量。通过中心复合设计（CCD）对这些选定的因素进行优化，以最大限度地提取 SLC。结果表明，最大限度地提取 SLC 的最佳条件为 pH 值 6.0、洗脱剂（乙腈）体积 300μL、吸附剂 10mg 和超声时间 6min。在优化条件下，SLC 的线性良好，范围为 30 至 4000ngmL，相关系数（R）为 0.99。检测限（LOD）为 2.50ngmL，两个加标水平的回收率范围为 97.37%至 103.21%，相对标准偏差（RSD）小于 4.50%（n=15）。增强因子（EF）为 81.91。结果表明，UAE 与 DNSPME 的结合是一种测定水样和尿样中 SLC 的合适方法。
