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Application of a tandem air-agitated liquid–liquid microextraction technique based on solidification of floating organic droplets as an efficient extraction method for determination of cholesterol-lowering drugs in complicated matrices

机译:一种串联气液微萃取技术的应用基于浮动有机液滴的凝固作为复杂基质中胆固醇降解药物的有效提取方法

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A simple and sensitive extraction method termed tandem air-agitated liquid–liquid microextraction based on solidification of floating organic droplets (TAALLME-SFO) is introduced. Based on this method, the three cholesterol-lowering drugs rosuvastatin, atorvastatin, and gemfibrozil, as the model analytes, were first extracted from a relatively large volume (10 mL) of an acidic donor phase into a small volume (105 μL) of an intermediate phase (a solidifiable organic solvent), and were then simply back-extracted into a smaller volume of a basic acceptor phase (55 μL) by micro-air-agitated liquid–liquid microextraction based on solidification of floating organic droplets (μ-AALLME-SFO). By performing this convenient extraction method, a high sample clean-up was obtained. The response surface methodology (RSM) combined with the desirability function (DF) was applied to the optimization of the effective parameters involved to reach the maximum extraction efficiency of the drugs. The pH values of the donor and acceptor phases and the volumes of the organic solvent (μL) and acceptor phase (μL) were obtained to be 3.0, 12, 105, and 55, respectively. Under the optimal experimental conditions, the TAALLME-SFO-HPLC-UV method provided good linearity for all the target analytes in the range of 2–3000 ng mL ~(?1) with coefficients of determination ( R ~(2) ) ≥ 0.995, and the intra-day and inter-day precisions varied in the ranges of 4.2–5.3 and 5.7–6.6, respectively. The limits of detection (LODs) were in the range of 0.5–1.0 ng mL ~(?1) . Consequently, this new microextraction technique was demonstrated to be suitable for the extraction and determination of the studied drugs in human plasma and wastewater samples.
机译:引入了一种简单敏感的提取方法,基于浮动有机液滴的凝固(Taallme-SFO)来称为串联气搅拌液 - 液微萃取。基于该方法,将三种胆固醇降低药物罗磺酰伐他汀,阿托伐他汀和Gemfibrozil作为模型分析物,首先从相对大的体积(10mL)的酸性供体相中提取成小体积(105μL)中间相(可变的有机溶剂),然后通过基于浮动有机液滴的凝固(μ-aallme),通过微空气搅拌液 - 液微萃取(μ-aallme -sfo)。通过进行这种方便的提取方法,获得了高样品清理。将与期望功能(DF)相结合的响应表面方法(RSM)对涉及的有效参数的优化,以达到药物的最大提取效率。将供体和受体相的pH值和有机溶剂(μl)和受体相(μl)的体积分别得到3.0,12,105和55。在最佳的实验条件下,Taallme-SFO-HPLC-UV方法为所有靶分析物提供良好的线性度,其所有目标分析物在2-3000ng ml〜(α1)的范围内,其中含量系数(R〜(2))≥0.995 ,日内和日内的血内诊断分别在4.2-5.3和5.7-6.6的范围内变化。检测限(LOD)的极限在0.5-1.0 ng ml〜(α1)的范围内。因此,该新的微萃取技术被证明适用于萃取和测定人血浆和废水样品中研究的药物。

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