Bovine Colostrum: Determination of Naturally Occurring Steroid Hormones by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)

Tiergesundheitsdienst Bayern e.V. , Senator-Gerauer-Strasse 23, 85586 Poing, Germany.
Journal of Agricultural and Food Chemistry (Impact Factor: 3.11). 02/2011; 59(4):1423-7. DOI: 10.1021/jf103751z
Source: PubMed

ABSTRACT The aim of this study was to collect further data about levels of endogenous hormones in foodstuffs derived from animal production. Because of expected higher concentrations of especially estrogens in colostrum compared to other foodstuffs, our investigation focused on this matrix. For evaluation of endogenous steroid hormones in separated colostrum (fat and defatted fraction) and colostrum powder, the relevant free and conjugated estrogens (estradiol-17β, estradiol-17α, estrone, and estriol) androgens (androstendione, 19nor-androstendione, 19nor-testosterone-17β, 19nor-testosterone-17α, testosterone-17β, and testosterone-17α), and progesterone were determined by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Upmost determined concentrations were found in the fat fraction, with 25.56 and 7.59 μg/L for estrone and androstendione, respectively. In defatted milk and colostrum powder, conjugated estrogens dominated, whereas total (free and conjugated) estrone (5.51 μg/L; 15.0 μg/kg) exceeded estradiol-17α (2.66 μg/L; 7.5 μg/kg) and estradiol-17β (2.28 μg/L; 3.3 μg/kg). Neither 19nor-steroids nor estriol were detected in colostrum fractions or processed colostrum.

  • [Show abstract] [Hide abstract]
    ABSTRACT: In this work, two mesoporous silicas functionalized with C18 groups (SM-C18 and SBA-15-C18) have been synthesized for their evaluation as stationary phases in SPE for the extraction and preconcentration of seven steroid hormones (estrone (E1), estradiol (E2), estriol (E3), ethinyl estradiol (EE2), diethylstilbestrol (DES), testosterone (T) and progesterone (P)) from milk. The characterization of both materials by diverse techniques such as TEM, SEM, thermogravimetric analysis (TGA), X-ray diffraction (XRD) and adsorption-desortion isotherms, showed that the mesoporous silicas had a high surface area, high pore volume and a homogeneous distribution of the pores and that both silicas presented a similar degree of functionalization. An analytical methodology for the simultaneous separation of the seven selected steroids by HPLC-DAD was developed. Both silicas were evaluated as stationary phases in SPE for the extraction of the steroid hormones from milk. This HPLC-DAD method was applied to the analysis of all extracts obtained in the SPE experiments, showing that from the two synthetized mesoporus silicas, SBA-15-C18 silica enabled the extraction of the seven compounds with recoveries between 88 and 108 % for all except for E3 for which a recovery of 62 % was obtained. The analytical characteristics of this methodology were evaluated, showing good precision and linearity (R20.994) for all analytes. The comparison of the results obtained with this silica and those obtained with commercial C18 particles and with some other commercial cartridges usually employed in the extraction of steroids showed that SBA-15-C18 silica was able to extract the seven steroids with higher recovery values. This article is protected by copyright. All rights reserved
    Electrophoresis 06/2014; 35(11). DOI:10.1002/elps.201300509 · 3.16 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: The occasional presence of relatively high amounts of natural estrogens in milk and milk derivatives and the abusive or illegal use of synthetic estrogens in dairy practices have become causes for concern, since intake of these hormones is associated with illnesses or disorders. Development of methodologies that confirm or deny the presence of natural and synthetic estrogens, their metabolites and other compounds with estrogenic activity is very important. This article provides an overview of chromatographic methods for the analysis of these compounds in milk samples and dairy products.
    TrAC Trends in Analytical Chemistry 03/2013; 44:58-77. DOI:10.1016/j.trac.2012.10.013 · 6.61 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: In this work, a simple and fast sample pretreatment method was proposed for determination of steroid hormones in fish tissues by coupling dynamic microwave-assisted extraction with salting-out liquid-liquid extraction. The steroid hormones were successively extracted with acetonitrile and water under the action of microwave energy. Subsequently, the extract was separated into an acetonitrile phase and an aqueous phase with ammonium acetate. The acetonitrile phase containing the target analytes was concentrated and determined by LC-MS/MS. The limits of detection for the steroid hormones were in the range of 0.03-0.15 ng g(-1). This method was successfully applied to analyze seven kinds of fish tissues, and the recoveries of the steroid hormones for the spiked samples were in the range of 75.3 ± 4.9% to 95.4 ± 6.2%. Compared with the traditional method, the proposed method could reduce the consumption of the organic solvent, shorten the sample preparation time, and increase the sample throughput.
    Journal of Agricultural and Food Chemistry 09/2012; 60(41):10343-51. DOI:10.1021/jf303124c · 3.11 Impact Factor