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首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Determination of deferasirox in human plasma by short-end injection and sweeping with a field-amplified sample stacking and micellar electrokinetic chromatography
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Determination of deferasirox in human plasma by short-end injection and sweeping with a field-amplified sample stacking and micellar electrokinetic chromatography

机译:短时进样并通过场放大样品堆积和胶束电动色谱法扫描测定人血浆中的地拉西罗

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A field-amplified sample stacking-sweeping micellar electrokinetic chromatography with short-end injection was established for determination of deferasirox (DFX) in plasma. DFX was extracted from plasma and reconstituted with deionized water (lower conductivity solution). Capillary (effective length, 10 cm) was filled with background electrolyte (40 mM phosphate buffer, pH 4.5, containing 20% methanol). After sample loading from outlet end at 5 psi for 15 s, separation was carried out by applying high voltage at 15 kV for 10 min. Sodium dodecyl sulfate (SDS) was used to sweep DFX for enhancing sensitivity. The optimal CE separation conditions were 40 mM phosphate buffer at pH 4.5 containing 100 mM SDS and 20% methanol. The analysis time was about 3.5 min for DFX. The calibration curve of DFX was ranged from 1 to 20 mu g/ml. The linearity (r) was more than 0.998. RSD and RE in intra- and inter-day assays were all below 12.14%. The limit of detection (LOD, S/N = 3) for DFX was 0.31 mu g/ml. The sensitivity enhancement factor between sweeping-FASS MEKC and capillary zone electrophoresis is 3.3. Finally, the method was applied for determination of DFX in beta-thalassemia patients. (C) 2016 Elsevier B.V. All rights reserved.
机译:建立了带有短时进样的场放大样品堆积扫描胶束电动色谱法,用于测定血浆中的地拉罗司(DFX)。从血浆中提取DFX,并用去离子水(电导率较低的溶液)重构。用背景电解质(40 mM磷酸盐缓冲液,pH 4.5,包含20%的甲醇)填充毛细管(有效长度,10 cm)。从出口端以5 psi的压力加载样品15 s后,通过施加15 kV的高压10分钟进行分离。十二烷基硫酸钠(SDS)用于清扫DFX以增强灵敏度。最佳的CE分离条件是pH值为4.5的40 mM磷酸盐缓冲液,其中含有100 mM SDS和20%甲醇。 DFX的分析时间约为3.5分钟。 DFX的校准曲线范围为1至20μg / ml。线性度(r)大于0.998。日内和日间分析的RSD和RE均低于12.14%。 DFX的检出限(LOD,S / N = 3)为0.31μg / ml。扫频FASS MEKC和毛细管区带电泳之间的灵敏度增强因子为3.3。最后,该方法用于测定β地中海贫血患者的DFX。 (C)2016 Elsevier B.V.保留所有权利。

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