NDLI: Analysis of Iodothyronines in Dietary Supplements Containing Dried Thyroid by HPLC Using a Pre-column Derivative

Content Provider	Springer Nature Link
Author	Sawabe, Yoshiyuki Tagami, Takaomi Doi, Takahiro Yamasaki, Katsuhiro Taguchi, Shuzo
Copyright Year	2011
Abstract	A new method to determine the iodothyronines, 3,3′,5-triiodo-L-thyronine (T3), 3,3′,5,5′-tetraiodo-L-thyronine (L-thyroxine, T4), and 3,3′,5′-triiodo-L-thyronine (reverse-T3, rT3), in dietary supplements containing dried thyroid by high-performance liquid chromatography was developed using a pre-column derivative with 4-fluoro-7-nitrobenzofurazan (NBD-F) without using LC/MS. T3, T4, and rT3 were released from dried thyroid in dietary supplements by using protease. The protease reaction was finished in 18 h at 37 °C. Iodothyronines released from dried thyroid were treated on a polyvinylpolypyrrolidone (PVPP) column. Iodothyronines adsorbed on PVPP were eluted with 60% acetonitorile. Iodothyronines present in the eluate from the PVPP column were then derivatized with NBD-F. The reaction of iodothyronines with NBD-F was completed in 30 min at 60 °C. These derivatives were measured by HPLC using an octadecylsilane column with a fluorescence detector. Phosphoric acid (0.1%) was added to 630 ml of acetonitrile to a final volume of 1,000 ml, and the mixture was used as the mobile phase. The excitation wavelength on the fluorescence detector was 470 nm, and the emission wavelength was 530 nm. The linearity of iodothyronines as a coefficient of the correlation value was 0.999, and the quantitation limit of iodothyronines was 0.001 μg/ml. The results confirmed that dried thyroid was added to seven dietary supplements. The recovery rate was in the range of 80.8–104.6%, 81.4–103.7%, and 82.2–104.5% for T3, T4, and rT3, respectively. Previously, dried thyroid in dietary supplements was examined by the combination of measuring T3 and T4 by LC/MS and confirmation of epithelial nuclei forming follicles by a microscope. However, microscopic confirmation of epithelial nuclei forming follicles can be complicated by physical alteration during dietary supplement processing. We suggest that the present of dried thyroid in dietary supplements can be confirmed by detecting rT3 without a microscope.
Starting Page	1033
Ending Page	1039
Page Count	7
File Format	PDF
ISSN	19369751
Journal	Food Analytical Methods
Volume Number	5
Issue Number	5
e-ISSN	1936976X
Language	English
Publisher	Springer-Verlag
Publisher Date	2011-12-03
Publisher Place	New York
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	3,3′,5-Triiodo-L-thyronine Thyroxine 4-Fluoro-7-nitrobenzofurazan Polyvinylpolypyrrolidone Thyroid HPLC Analytical Chemistry Chemistry/Food Science Microbiology Food Science
Content Type	Text
Resource Type	Article
Subject	Analytical Chemistry Safety Research Safety, Risk, Reliability and Quality Applied Microbiology and Biotechnology Food Science

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