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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

Determination of thyroid hormones in plasma samples by high performance liquid chromatograph/diode array detector/electrospray ionization mass spectrometer

Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2007, v.20 no.5, pp.424-433



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Abstract

An analytical method for the determination of thyroid hormones in plasma samples has been studied by solid-phase extraction and high-performance liquid chromatography/diode array detector (DAD)/electrospray ionization (ESI)-mass spectrometer. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 250 mm length, particle size <TEX>$5{\mu}m$</TEX>) with ammonium formate buffer and acetonitrile. In addition, these compounds were confirmed by UV spectra and ESI-mass Spectra. The extraction recoveries of thyroid hormones in the plasma sample (at pH 3) were in the range of 74.5-115.7 % with solid-phase extraction by C18, followed by elution with 4 mL of methanol. The calibration curves showed good linearity with the correlation coefficients (<TEX>$r^2$</TEX>) varying from 0.9939 to 0.9978 and the detection limits of all analytes were obtained in the range of 20-50 ng/mL (38.1-162.8 pmol/mL). As a result, thyroxine was found in the range of 50.98-112.97 ng/mL in normal plasma samples.

keywords
thyroid hormones, HPLC/DAD/ESI-MS, SPE, plasma


Reference

1

O, (1974) “Handbook of physiology,

2

안세영, (2004) 갑상선 클리닉, 성보사

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