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电纺聚对苯二甲酸乙二醇酯/氧化石墨烯纳米纤维膜结合高效液相色谱法分离和测定人血浆中的他莫昔芬。

Electrospun polyethylene terephthalate/graphene oxide nanofibrous membrane followed by HPLC for the separation and determination of tamoxifen in human blood plasma.

机构信息

Department of Chemistry, Faculty of Science, University of Tehran, Tehran, Iran.

出版信息

J Sep Sci. 2017 Sep;40(17):3383-3391. doi: 10.1002/jssc.201700312. Epub 2017 Jul 21.

DOI:10.1002/jssc.201700312
PMID:28664592
Abstract

An electrospun polyethylene terephthalate/graphene oxide nanofibrous mat was fabricated and used as an effective and novel membrane for the solid-phase extraction of tamoxifen in human blood plasma samples before detection by high-performance liquid chromatography. The membrane was characterized by some identification techniques, such as FTIR spectroscopy, X-ray diffraction, and scanning electron microscopy. The effective variables of the extraction procedure including desorption condition (type and volume of the eluent), adsorbent dose, pH of sample solution, salt concentration, and sample loading time were investigated and their optimum values were obtained using one factor at a time methodology. Under the optimized conditions, the results showed wide linear concentration range of 5-2000 ng/mL with a determination coefficient of 0.992. The limits of detection and limits of quantification were 1.3 and 5.0 ng/mL, respectively. The intra-day and inter-day precisions were 3.4 and 4.6%, respectively. The method was successfully applied to determination of tamoxifen in the blood plasma samples and satisfactory relative recoveries (92.6-98.3 %) were achieved.

摘要

制备了一种静电纺丝的聚对苯二甲酸乙二醇酯/氧化石墨烯纳米纤维垫,并将其用作高效、新颖的固相萃取膜,用于高效液相色谱检测前人血浆样品中的他莫昔芬。采用傅里叶变换红外光谱、X 射线衍射和扫描电子显微镜等鉴定技术对膜进行了表征。采用单因素法考察了萃取过程的有效变量,包括解吸条件(洗脱剂的类型和体积)、吸附剂剂量、样品溶液 pH 值、盐浓度和样品加载时间,并获得了最佳值。在优化条件下,结果表明该方法的线性浓度范围为 5-2000ng/mL,相关系数为 0.992。检测限和定量限分别为 1.3 和 5.0ng/mL。日内和日间精密度分别为 3.4%和 4.6%。该方法成功应用于测定血浆样品中的他莫昔芬,获得了令人满意的相对回收率(92.6-98.3%)。

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