Synergistic integration of μ-SPE and ammoniated adduct-based MRM for sensitive UPLC-MS/MS quantification of PEG1000: a comparative study against in-source CID and application to zebrafish tissue distribution.

Authors

Xinyue Zhou, Sufei Duan, Yuye Lou, Yue Deng, Shuang Feng, Jiale Liu, Jiarui Zhang, Yalin Xi, Meiyun Shi, Lei Yin

Published in

Analytical and bioanalytical chemistry. Jul 13, 2026. Epub Jul 13, 2026.

Abstract

A sensitive UPLC-MS/MS method was developed and validated for quantifying polyethylene glycol 1000 (PEG1000) in zebrafish tissues, featuring a systematic comparison of two MS acquisition strategies. Through comprehensive optimization, the ammonium adduct [M+NH₄]⁺ of the representative 18-EO oligomer (m/z 828.5) was selected as the precursor ion, achieving approximately fourfold higher signal intensity than [M+H]⁺. Critically, the conventional high declustering potential in-source CID approach monitoring fragment ions was outperformed by the optimized MRM method monitoring the intact ammoniated precursor, which demonstrated 2.7-fold signal enhancement and superior selectivity. The integration of micro-solid-phase extraction (μ-SPE) further improved method performance, yielding 1.5-fold signal gain and markedly reduced matrix effects compared to conventional protein precipitation. The fully validated method exhibited excellent linearity (0.5-50 μg/mL, r > 0.995), accuracy, precision, and stability. Application to zebrafish tissue distribution studies revealed pronounced organ-specific accumulation following aqueous exposure to 200 μg/mL PEG1000, with highest concentrations in intestine tissue exhibiting a time-dependent increase, followed by muscle, while muscle maintained consistently low levels. This analytical platform, synergistically combining μ-SPE cleanup and ammoniated adduct-based MRM, offers superior sensitivity over in-source CID approaches and provides a practical framework for polymer bioanalysis, yielding critical insights into the in vivo fate of PEG-based compounds. The key novelties of this work are the following: (i) the first systematic comparison between ammoniated adduct MRM and high-DP in-source CID for PEG1000 quantification; (ii) the introduction of μ-SPE for sample preparation in zebrafish tissues, achieving 1.5-fold signal enhancement; and (iii) the successful application of this platform to reveal organ-specific accumulation patterns of PEG1000.

PMID:
42439928
Bibliographic data and abstract were imported from PubMed on 13 Jul 2026.

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