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Ultrasound-promoted dispersive micro solid-phase extraction of trace anti-hypertensive drugs from biological matrices using a sonochemically synthesized conductive polymer nanocomposite

机译:使用SOOCOOCHIMY合成的导电聚合物纳米复合材料从生物基质中促进微量抗高血压药物的超声波抗高血压药物

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In this work, a rapid and efficient procedure named ultrasound meliorated dispersive micro solid-phase extraction followed by high performance liquid chromatography-ultra violet detection (US-D-mu SPE-HPLC-UV) was developed for the pre-concentration of the main trace anti-hypertensive drugs in complex matrices. The basis of this procedure was a polypyrrole-sodium dodecylbenzenesulfonate/zinc oxide (PPy-DBSNa/ZnO) nanocomposite. It was readily synthesized by the impressive way of in situ sonochemical oxidative polymerization in the presence of some additives such as FeCl3 and DBSNa, ultimately leading to the effective coating of PPy on the ZnO nanoparticle cores. Characterization of the proposed nanosorbent was performed by different techniques such as FESEM, XRD,EDX, and TGA, confirming the high quality and proper physico-chemical properties of the proposed sorbent. In order to better investigate the input variables, the central composite design (CCD) combined with the desirability function (DF) was utilized. The enriched optimum conditions consisted of the initial pH value of 11.8, 15 mg of the PPy-DBSNa/ZnO nanocomposite, a sonication time of 4.6 min, and 100 mu L of methanol, resulting in maximum responses at a relatively low extraction time with a logical DF. Under the optimum conditions, good linearity (5-5000, 2.5-3500, and 2.5-3000 ng mL(-1) for metoprolol, propranolol, and carvedilol, respectively, with the correlation of determinations (R(2)s) higher than 0.99), low limits of detection (LODs) (0.8-1.5 ng mL(-1)), proper repeatabilities (relative standard deviation values (RSDs) below 6.3%, n = 3), reasonable enrichment factors (EFs) (60-72), and good extraction recoveries (ERs) (higher than %75) were obtainable. These appropriate validations corroborated a good effectiveness of ultrasonic waves in the achievement of a supreme solid phase as well as a facile and efficient microextraction of the low therapeutic concentrations in human plasma and urine samples. (c) 2017 Published by Elsevier B.V.
机译:在这项工作中,开发了一种快速高效的方法,称为超声化分散微固相提取,然后开发出高性能液相色谱 - 超紫色检测(US-D-MU SPE-HPLC-UV),用于主要的主要浓度复杂矩阵中的痕量抗高血压药物。该方法的基础是聚吡咯 - 十二烷基苯磺酸盐/氧化锌(PPY-DBSNA / ZnO)纳米复合材料。在某些添加剂如FECL3和DBSNA存在下,通过原位的氧化聚合的令人印象深刻的方式易于合成,最终导致ZnO纳米粒子芯上的PPY的有效涂层。所提出的纳米吸船剂的表征通过不同的技术,例如FESEM,XRD,EDX和TGA进行,确认所提出的吸附剂的高质量和适当的物理化学性质。为了更好地研究输入变量,利用与期望功能(DF)结合的中央复合设计(CCD)。富集的最佳条件包括11.8,15mg PPY-DBSNA / ZnO纳米复合材料的初始pH值,4.6分钟的超声处理时间和100μl甲醇,导致在相对低的提取时间下的最大响应逻辑DF。在最佳条件下,良好的线性度(5-5000,2.5-3500和2.5-3000ng ml(-1)分别用于富含托洛尔,普萘洛尔和卡维地洛(R(2))高于0.99),低检测限(LOD)(LODS)(0.8-1.5 ng ml(-1)),适当的重组(相对标准偏差值(RSD)低于6.3%,n = 3),合理的富集因子(EFS)(60- 72),可获得良好的提取回收(ERS)(高于%75)。这些适当的验证证实了超声波在实现最高固相方面的良好效果,以及人血浆和尿液样品中低治疗浓度的容易和有效的微直接。 (c)2017年由Elsevier B.V发布。

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