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Solid-phase extraction combined with dispersive liquid-liquid microextraction as an efficient and simple method for the determination of carbamazepine in biological samples

机译:固相萃取与分散液-液微萃取相结合是测定生物样品中卡马西平的一种有效而简便的方法

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摘要

An analytical method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), is established to determine carbamazepine in biological fluids and water samples. After concentration and purification of the samples in SPE C_(18) sorbent, 1.5 mL of acetonitrile containing 60.0 uL of chloroform was injected into 5.0 mL pure water. After extraction and centrifuging, the sedimented phase was evaporated and the residue was dissolved in 30 uL methanol and injected into the HPLC system. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, are studied and optimized. The new method (SPE-DLLME) provides detection limits of 0.8 μg L~(-1) and 1.7 μg L~(-1) in urine and plasma samples, respectively. The calibration graphs are linear in the range of 2.5-500 μg L~(-1) and 5.0-500 μg L~(-1) in urine and plasma, respectively. The results show that SPE-DLLME is a suitable method for the determination of carbamazepine in biological and water samples.
机译:建立了一种固相萃取结合液-液微分散萃取(SPE-DLLME)的分析方法,用于测定生物流体和水样品中的卡马西平。在SPE C_(18)吸附剂中浓缩和纯化样品后,将含有60.0 uL氯仿的1.5 mL乙腈注入5.0 mL纯水中。萃取并离心后,将沉淀相蒸发,并将残留物溶于30 uL甲醇中,然后注入HPLC系统。研究并优化了一些重要的提取参数,例如样品溶液的流速,样品的pH值,提取和分散溶剂的类型和体积以及盐的添加量。新方法(SPE-DLLME)在尿液和血浆样品中的检出限分别为0.8μgL〜(-1)和1.7μgL〜(-1)。尿液和血浆中的校准曲线分别在2.5-500μgL〜(-1)和5.0-500μgL〜(-1)范围内呈线性关系。结果表明,SPE-DLLME是测定生物和水样品中卡马西平的合适方法。

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