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Microwave-Assisted Extraction Coupled with Single Drop Microextraction and High-Performance Column Liquid Chromatography for the Determination of Trace Estrogen Adulterants in Soybean Isoflavone Dietary Supplements

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A sensitive and accurate method consisting of microwave-assisted extraction (MAE) coupled with single drop microextraction (SDME) and HPLC was developed for the determination of four trace estrogen adulterants, including estriol (E3), estradiol (E2), ethinyl estradiol (EE), and estrone (E1), in different soybean dietary supplements. The samples were extracted by MAE; the extracts were cleaned up and enriched by SDME, and then analyzed by HPLC. The conditions of MAE were optimized, and the effects of solvent and extraction time in SDME on the enrichment capacity were studied. The enrichment factors of E3, E2, EE, and E1 under the optimized conditions were 247-, 335-, 316-, and 319-fold, respectively. The linear range of the MAE-SDME-HPLC method ranged from 5.0 to 180.0 g/L, and the detection limit from 1.1 to 1.2 g/L. The RSD ranged from 7.9 to 9.6. Three soybean dietary supplements, including oral liquid, capsule, and tablet forms, were analyzed. The spike recovery was more than 70, with RSD lower than 13.2. It was shown that the proposed method was accurate, sensitive, and suitable for the determination of trace analytes in complex samples.
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Document Type: Research Article

Affiliations: Sun Yat-Sen University, School of Chemistry and Chemical Engineering, Guangzhou 510275, People's Republic of China.

Publication date: May 1, 2010

More about this publication?
  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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