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

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

doi:10.1007/s10337-022-04178-4

Cited by 3 publications

(4 citation statements)

References 47 publications

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“…In this latter study, the RE of E2 was 97.6%, with LOD and LOQ values of 6.71 and 22.1 ng mL –1 , and no quantitative analysis was obtained from serum (Table S4). A similar situation was described in another work, where poly(methacrylic acid/3-acrylamidophenylboronic acid- co -ethylene glycol dimethacrylate) monolith was used for offline extraction of estrogens, including E2, resulting in 96.4% RE and LOD and LOQ values at 37 and 100 ng L –1 , respectively . In this case as well, quantification of a real-world serum sample could not be achieved.…”

Section: Resultsmentioning

confidence: 67%

“…A similar situation was described in another work, where poly(methacrylic acid/3-acrylamidophenylboronic acidco-ethylene glycol dimethacrylate) monolith was used for offline extraction of estrogens, including E2, resulting in 96.4% RE and LOD and LOQ values at 37 and 100 ng L −1 , respectively. 32 In this case as well, quantification of a real-world serum sample could not be achieved. In the case of the method described in this work, the limits were experimentally determined rather than calculated from the very low S/N in the MRM analysis.…”

Section: Analyticalmentioning

confidence: 97%

“…To the best of our knowledge, online systems for the extraction and cleanup of estrogens, including E2, were described for other matrices, such as urine, 26 water, 27,28 and food (milk and shrimp) 29 but not for serum. For serum IT-SPME techniques were developed employing only offline methods, 32 including one with the potential for automation. 30 In this latter study, the RE of E2 was 97.6%, with LOD and LOQ values of 6.71 and 22.1 ng mL −1 , and no quantitative analysis was obtained from serum (Table S4).…”

Section: Analyticalmentioning

confidence: 99%

“…MIP was used for the extraction of six estrogenic compounds from milk . Additionally, a poly(methacrylic acid/3-acrylamidophenylboronic acid- co -ethylene glycol dimethacrylate) monolith was used for extraction of six estrogens from urine and serum; these reports are significant as they demonstrate the feasibility of sample preparation, including complex biofluids as serum, through IT-SPME. However, automation remains challenging.…”

mentioning

confidence: 99%

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Preparation of Monolith for Online Extraction and LC–MS Analysis of β-Estradiol in Serum Via a Simple Multicomponent Reaction

Cerrato,

Aita,

Cavaliere

et al. 2024

Anal. Chem.

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Multicomponent reactions offer efficient and environmentally friendly strategies for preparing monoliths suitable for applications in analytical chemistry. In the described study, a multicomponent reaction was utilized for the one-pot miniaturized preparation of a poly(propargyl amine) polymer inside commercial silica-lined PEEK tubing. The reaction involved only small amounts of reagents and was characterized by atom economy. The resulting monolithic column was incorporated into an autosampler system for the online extraction and cleanup of β-estradiol from human serum. Sample pretreatment was simplified to a simple dilution with methanol and centrifugation to remove proteins. The resulting platform included LC−MS analysis in multiple reaction monitoring for quantitative analysis of β-estradiol. The method was validated in serum, demonstrating practical applicability for the monitoring of fertile women. Recoveries were above 94%, and LOD and LOQ values at 0.008 and 0.18 ng mL −1 , respectively. The developed platform proved to be competitive with previous methods for solidphase microextraction of β-estradiol in serum, with comparable recovery and sensitivity but with the advantage of nearly complete automation. The environmental impact of the process was evaluated as acceptable due to the miniaturization of the monolith synthesis and the automation of extraction. The drawback associated with the LC−MS technique can be reduced by the inclusion of additional analytes in a single investigation. The work demonstrates that multicomponent reactions are versatile, economical, and possibly a green methodology for producing reversed-phase and mixed-mode sorbents, enabling miniaturization of the entire analytical procedure from the preparation of extraction sorbents to analysis.

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Section: Resultsmentioning

confidence: 67%

Section: Analyticalmentioning

confidence: 97%