Development of an Efficient Solid-Phase Microextraction Monolithic Column for the Analysis of Estrogens in Human Urine and Serum Samples

IF 1.2 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS Chromatographia Pub Date : 2022-06-24 DOI:10.1007/s10337-022-04178-4

Qianchun Zhang, Yutong Wang, Bingnian Yang, Linchun Bao, Yun Wu, Xingyi Wang

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Abstract

Estrogen plays a crucial role in various stages of human development and is present in the human body at trace level; therefore, an efficient strategy for the quantitative analysis of trace estrogens is required. However, this analysis is complicated by the presence of extremely complex biological matrices. To address this challenge, a novel method based on monolithic column solid-phase microextraction and ultra-high-performance liquid chromatography-tandem mass spectrometry was developed for the sensitivity analysis of six estrogens: β-estradiol, α-estradiol, 17α-ethynylestradiol, estrone, diethylstilbestrol, and hexestrol, in human urine and serum samples. The method exhibits a low limit of detection (8.6–37 ng L⁻¹), with wide linear ranges (0.10–25 μg L⁻¹) for each analyte and remarkable correlation coefficients (R² = 0.9953–0.9995). The developed method was successfully used to detect estrogens in urine and serum samples. The six analytes were satisfactorily recovered between 76.2 and 107% with relative standard deviations ranging from 2.5 to 8.3% (n = 3). The results demonstrated that the developed method, based on a poly(methacrylic acid/3-acrylamidophenylboronic acid-co-ethylene glycol dimethacrylate) monolithic column, is an effective enrichment approach toward the analysis of trace estrogens in human urine and serum samples.

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高效固相微萃取整体柱的研制用于分析人尿和血清中雌激素

雌激素在人类发育的各个阶段起着至关重要的作用，在人体中以微量水平存在;因此，需要一种有效的方法对微量雌激素进行定量分析。然而，这种分析是复杂的存在极其复杂的生物基质。为了解决这一挑战，我们建立了一种基于整体柱固相微萃取和超高效液相色谱-串联质谱的新方法，用于分析人类尿液和血清样品中6种雌激素:β-雌二醇、α-雌二醇、17α-乙炔雌二醇、雌酮、己烯雌酚和己烯雌酚的敏感性。该方法检出限低(8.6 ~ 37 ng L−1)，线性范围宽(0.10 ~ 25 μ L−1)，相关系数显著(R2 = 0.9953 ~ 0.9995)。该方法已成功地用于检测尿液和血清样品中的雌激素。6种分析物的回收率为76.2 ~ 107%，相对标准偏差为2.5 ~ 8.3% (n = 3)。结果表明，基于聚(甲基丙烯酸/3-丙烯酰胺苯基硼酸-共乙二醇二甲基丙烯酸酯)整体柱的富集方法是一种有效的分析人体尿液和血清样品中痕量雌激素的富集方法。图形抽象

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来源期刊

Chromatographia 化学-分析化学

CiteScore

3.40

自引率

5.90%

发文量

103

审稿时长

2.2 months

期刊介绍： Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.