分散液液微萃取-高效液相色谱法测定人尿中诺龙和睾酮的含量

IF 16.4 1区化学 Q1 CHEMISTRY, MULTIDISCIPLINARY

Accounts of Chemical Research Pub Date : 2023-01-20 DOI:10.1556/1326.2021.00972

M. Rezaee

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引用次数: 0

摘要

建立了分散液液微萃取(DLLME) -高效液相色谱-紫外检测法提取测定人尿中诺龙酮和睾酮的方法。以微升体积的氯仿和乙腈分别作为提取溶剂和分散溶剂。该方法的主要优点是萃取速度快、富集系数高、回收率高、重复性好，萃取溶剂量在µL级。仔细评估了几个变量(例如分散剂和萃取溶剂的类型和体积，离子强度等)对样品制备步骤性能的影响。在最佳条件下，两种方法在5 ~ 500 μ L−1范围内均呈线性关系，检出限均为2.5 μ L−1。诺龙和睾酮5次重复测量的相对标准偏差(rsd)分别为9.4%和8.8%。在25.0 μg L−1峰浓度下，诺龙酮和睾酮的相对回收率为86.4% ~ 98%。DLLME联合HPLC-UV是一种快速、简便、高效的测定人尿中诺龙和睾酮的方法。

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Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine

Dispersive liquid-liquid microextraction (DLLME) and high performance liquid chromatography – UV detection was presented for extraction and determination of nandrolone and testosterone in human urines. Chloroform at microliter volume level and acetonitrile were used as extraction and dispersive solvents, respectively. The main advantages of method are high speed, high enrichment factor, high recovery, good repeatability and extraction solvent volume at µL level. The influence of several variables (e.g. type and volume of disperser and extraction solvents, ionic strength, etc.) on the performance of the sample preparation step was carefully evaluated. Under the optimum conditions, the calibration graphs were linear in the range of 5–500 μg L−1 with detection limit of 2.5 μg L−1 for both of them. The relative standard deviation (R.S.D.s) for five replicate measurements of nandrolone and testosterone were 9.4% and 8.8%, respectively. The relative recoveries of nandrolone and testosterone in urine sample at spiking level of 25.0 μg L−1 are ranged between 86.4% and 98%. DLLME combined with HPLC-UV is a fast, simple and efficient method for the determination of nandrolone and testosterone in human urines.

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来源期刊

Accounts of Chemical Research 化学-化学综合

CiteScore

31.40

自引率

1.10%

发文量

312

审稿时长

2 months

期刊介绍： Accounts of Chemical Research presents short, concise and critical articles offering easy-to-read overviews of basic research and applications in all areas of chemistry and biochemistry. These short reviews focus on research from the author’s own laboratory and are designed to teach the reader about a research project. In addition, Accounts of Chemical Research publishes commentaries that give an informed opinion on a current research problem. Special Issues online are devoted to a single topic of unusual activity and significance. Accounts of Chemical Research replaces the traditional article abstract with an article "Conspectus." These entries synopsize the research affording the reader a closer look at the content and significance of an article. Through this provision of a more detailed description of the article contents, the Conspectus enhances the article's discoverability by search engines and the exposure for the research.