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首页> 外文期刊>Journal of the Brazilian Chemical Society >Determination of glucocorticoids using cosurfactants ultrasonic- thermostatic-assisted cloud point extraction followed by high performance liquid chromatography
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Determination of glucocorticoids using cosurfactants ultrasonic- thermostatic-assisted cloud point extraction followed by high performance liquid chromatography

机译:辅助表面活性剂超声-恒温辅助浊点萃取-高效液相色谱法测定糖皮质激素

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摘要

A novel approach, cosurfactants ultrasonic-thermostatic-assisted cloud point extraction (CUS-CPE) combined with high performance liquid chromatography and ultraviolet detection (HPLC-UV) is developed for the analysis of glucocorticoids (beclometasone dipropionate (BD), hydrocortisone butyrate (HB) and nandrolone phenylpropionate (NPP)) in human urine samples. In this study, four different cloud point extraction (CPE) systems are discussed, including DC-193-nonanoic acid, DC-193-sodium sulfate, DC-193-lauric acid and the classic Triton X-100 sulfate systems. Among them, DC-193-sodium sulfate and the classic Triton X-100 sulfate systems has been studied in the past few years. Comparing with the first two systems, DC-193-nonanoic acid system had a lower cloud point (CP), little UV absorbance and it is less damaging to the column of three glucocorticoids in same surfactant concentration which was required for application as a pre-concentration process prior to HPLC. Phase diagrams were used to study the cavitation and mass transfer behaviors of the two phases on micelles of polyether type organic silicon surfactant, PEG-12 dimethicone (DC-193).The volumes of surfactant-rich phase obtained were very small (the enrichment factor (EF) was 35), which was much smaller and had a quick phase separating speed than that of Triton X-100 in the same surfactant concentration. Linearity was investigated from 1 to 350 ng mL~(-1). The limits of detection (LOD) thus estimated were 1.29 for BD, 2.67 for HB and 3.33 ng mL ~(-1) for NPP, respectively. In proposed CPE step is rapid and effective to obtain recovery of three glucocorticoids higher than 85%, which is similar or better than literature reported data. The method was shown to be selective, linear, precise and reproducible and successfully applied for the analysis of glucocorticoids in human urine samples.
机译:开发了一种新方法,将辅助表面活性剂超声-恒温辅助浊点提取(CUS-CPE)与高效液相色谱和紫外检测(HPLC-UV)相结合,用于分析糖皮质激素(倍氯米松双丙酸酯(BD),氢化可的松丁酸酯(HB) )和人类尿液样本中的苯丙酸诺龙(NPP))。在这项研究中,讨论了四种不同的浊点萃取(CPE)系统,包括DC-193-壬酸,DC-193-硫酸钠,DC-193-月桂酸和经典的Triton X-100硫酸盐系统。其中,过去几年已经研究了DC-193-硫酸钠和经典的Triton X-100硫酸盐系统。与前两个系统相比,DC-193-壬酸系统具有较低的浊点(CP),较低的紫外线吸收率,并且在相同表面活性剂浓度下对三种糖皮质激素的色谱柱造成的损害较小,这是应用前的要求。 HPLC之前的浓缩过程。用相图研究了两相在聚醚型有机硅表面活性剂PEG-12二甲聚硅氧烷(DC-193)的胶束上的空化和传质行为,所得表面活性剂富集相的体积很小(富集因子(EF)为35),在相同的表面活性剂浓度下,它比Triton X-100小得多,并且具有较快的相分离速度。线性范围为1至350 ng mL〜(-1)。如此估计的检出限(LOD)对于BD为1.29,对于HB为2.67,对于NPP为3.33 ng mL〜(-1)。在提出的CPE步骤中,快速有效地获得了三种回收率高于85%的糖皮质激素,这与文献报道的数据相似或更好。该方法具有选择性,线性,精确和可重现的特点,已成功用于人尿液中糖皮质激素的分析。

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