Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan, Hubei, China.
Anal Chim Acta. 2011 Mar 18;689(2):219-25. doi: 10.1016/j.aca.2011.01.045. Epub 2011 Jan 27.
In the present study, a three phase-based hollow fiber protected liquid-phase microextraction (HF-LPME) method combined with high-performance liquid chromatography (HPLC) for the determination of salicylates in environmental waters was developed. The HF-LPME procedure was optimized by an L(16)(4(5)) orthogonal array experimental design (OAD) with five factors at four levels. Under the optimal extraction condition (pHs of donor and receiving phases of 3.0 and 6.2, respectively, extraction time of 45 min, stirring speed of 1000 rpm, and salt addition of 20% (w/v)), salicylates could be determined in a linear range from 0.025 to 1.0 μg mL(-1) with a good correlation (r(2)>0.9930). The limits of detection (LODs) ranged between 0.6 ng mL(-1) and 1.2 ng mL(-1) for the target analytes. The relative standard deviations (RSDs) of intra-day and inter-day were in the range of 0.64-14.58% and 0.16-15.45%, respectively. This procedure afforded a convenient, sensitive, accurate and cost-saving operation with high extraction efficiency for the model analytes. The method was applied satisfactorily to the determination of salicylates in two environmental waters.
在本研究中，开发了一种基于三相的中空纤维保护液相微萃取（HF-LPME）方法，结合高效液相色谱（HPLC），用于测定环境水中的水杨酸盐。HF-LPME 程序通过 L(16)(4(5))正交数组实验设计（OAD）进行优化，具有五个因素和四个水平。在最佳萃取条件下（供体和受体相的 pH 值分别为 3.0 和 6.2，萃取时间为 45 分钟，搅拌速度为 1000 rpm，盐添加量为 20%（w/v）），水杨酸盐可以在 0.025 至 1.0 μg mL(-1)的线性范围内进行测定，具有良好的相关性（r(2)>0.9930）。目标分析物的检测限（LOD）范围在 0.6 ng mL(-1)至 1.2 ng mL(-1)之间。日内和日间的相对标准偏差（RSD）分别在 0.64%-14.58%和 0.16%-15.45%之间。该程序为模型分析物提供了一种方便、灵敏、准确且节省成本的操作，具有高萃取效率。该方法满意地应用于两种环境水中水杨酸盐的测定。
