Asfaram Arash, Ghaedi Mehrorang, Goudarzi Alireza
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.
Ultrason Sonochem. 2016 Sep;32:407-417. doi: 10.1016/j.ultsonch.2016.04.009. Epub 2016 Apr 7.
A simple, low cost and ultrasensitive method for the simultaneous preconcentration and determination of trace amount of auramine-O and malachite green in aqueous media following accumulation on novel and lower toxicity nanomaterials by ultrasound-assisted dispersive solid phase micro-extraction (UA-DSPME) procedure combined with spectrophotometric has been described. The Mn doped ZnS nanoparticles loaded on activated carbon were characterized by Field emission scanning electron microscopy (FE-SEM), particle size distribution, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) analyses and subsequently were used as green and efficient material for dyes accumulation. Contribution of experimental variables such as ultrasonic time, ultrasonic temperature, adsorbent mass, vortex time, ionic strength, pH and elution volume were optimized through experimental design, and while the preconcentrated analytes were efficiently eluted by acetone. Preliminary Plackett-Burman design was applied for selection of most significant factors and giving useful information about their main and interaction part of significant variables like ultrasonic time, adsorbent mass, elution volume and pH were obtained by central composite design combined with response surface analysis and optimum experimental conditions was set at pH of 8.0, 1.2mg of adsorbent, 150μL eluent and 3.7min sonication. Under optimized conditions, the average recoveries (five replicates) for two dyes (spiked at 500.0ngmL(-1)) changes in the range of 92.80-97.70% with acceptable RSD% less than 4.0% over a linear range of 3.0-5000.0ngmL(-1) for the AO and MG in water samples with regression coefficients (R(2)) of 0.9975 and 0.9977, respectively. Acceptable limits of detection of 0.91 and 0.61ngmL(-1) for AO and MG, respectively and high accuracy and repeatability are unique advantages of present method to improve the figures of merit for their accurate determination at trace level in complicated materials.
本文描述了一种简单、低成本且超灵敏的方法，通过超声辅助分散固相微萃取（UA-DSPME）程序结合分光光度法，在新型低毒性纳米材料上富集后，同时对水介质中痕量的金胺-O和孔雀石绿进行预富集和测定。负载在活性炭上的锰掺杂硫化锌纳米颗粒通过场发射扫描电子显微镜（FE-SEM）、粒度分布、X射线衍射（XRD）、傅里叶变换红外光谱（FT-IR）分析进行表征，随后用作绿色高效的染料富集材料。通过实验设计优化了超声时间、超声温度、吸附剂质量、涡旋时间、离子强度、pH值和洗脱体积等实验变量的影响，同时用丙酮有效地洗脱预富集的分析物。初步的Plackett-Burman设计用于选择最显著的因素，并通过中心复合设计结合响应面分析获得有关超声时间、吸附剂质量、洗脱体积和pH值等显著变量的主要和交互部分的有用信息，最佳实验条件设定为pH值8.0、1.2mg吸附剂、150μL洗脱剂和3.7分钟超声处理。在优化条件下，两种染料（加标浓度为500.0ngmL(-1)）的平均回收率（五次重复）在92.80-97.70%范围内，对于水样中AO和MG在3.0-5000.0ngmL(-1)的线性范围内，相对标准偏差（RSD%）小于4.0%，回归系数（R(2)）分别为0.9975和0.9977。AO和MG的检测限分别为0.91和0.61ngmL(-1)，以及高准确性和可重复性是本方法的独特优势，可提高在复杂材料中痕量水平准确测定的品质因数。
