Column-switching high-performance liquid chromatography electrospray mass spectrometry coupled with on-line of extraction for the determination of mono- and di- (2-ethylhexyl) phthalate in blood samples

Inoue, K.; Kawaguchi, M.; Okada, F.; Yoshimura, Y.; Nakazawa, H.

Analytical and Bioanalytical Chemistry 375(4): 527-533

2003


ISSN/ISBN: 1618-2642
PMID: 12610705
DOI: 10.1007/s00216-002-1709-9
Accession: 010345371

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Abstract
A novel method based on column-switching high-performance liquid chromatography-electrospray mass spectrometry (LC-MS) coupled with an on-line extraction column containing conjugated avidin has been developed for direct injection analysis of di(2-ethylhexyl) phthalate (DEHP) and its metabolite, mono(2-ethylhexyl) phthalate (MEHP), in blood samples. The sample preparation for on-line extraction involved the mixing of blood samples with internal standards, DEHP-d(4) and MEHP-d(4), in LC glass vials. A linear response was found for column-switching LC-MS when tests were conducted within the validated range of 25 to 1000 ng mL(-1) for DEHP and 5 to 1000 ng mL(-1) for MEHP, with correlation coefficients (r) greater than 0.999. In addition, the recoveries of DEHP and MEHP from human plasma were calculated by using this method with on-line extraction, yielding recoveries of up to 91.2% (RSD<5%). We measured the background levels of DEHP and MEHP in six human plasma samples from healthy volunteers and three fetal bovine serum samples for cell-line culture. DEHP and MEHP were not detected in all human plasma samples (N.D. is <25 ng mL(-1) for DEHP, and N.D. is <5.0 ng mL(-1) for MEHP). In contrast, high DEHP contamination of commercially available fetal bovine serum samples was found by this method.

Column-switching high-performance liquid chromatography electrospray mass spectrometry coupled with on-line of extraction for the determination of mono- and di-(2-ethylhexyl) phthalate in blood samples