Hydrophilic interaction liquid chromatography-tandem mass spectrometry determination of estrogen conjugates in human urine.

作者: Feng Qin , Yuan-Yuan Zhao , Michael B. Sawyer , Xing-Fang Li

DOI: 10.1021/AC702613K

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摘要: We report a hydrophilic interaction liquid chromatography (HILIC) separation with tandem mass spectrometry (MS) detection method for analysis of seven urinary estrogen conjugates. HILIC employing mobile phase high organic solvent content resulted in enhanced electrospray ionization efficiency and MS sensitivity compared reversed-phase (RP) LC−MS methods. Solid-phase extraction (SPE) was used to further improve the limit eliminate interferences urine samples. No hydrolysis or derivatization required sample pretreatment. This SPE/HILIC−MS/MS provided limits quantification (LOQs at S/N = 10) conjugates ranging from 2 1000 pg/mL only 1 mL sample, representing an improvement order magnitude over RPLC methods previously reported. linear dynamic range 3 orders magnitude, recovery 92−109%, intraday accuracy 84−109%, precision 1−14%,...

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