Simultaneous determination of 30 hormones illegally added to anti-ageing functional foods using UPLC-MS/MS coupled with SPE clean-up

Abstract

A novel analytical method employing solid-phase extraction (SPE) coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 30 hormones in anti-ageing functional foods (capsules, powders and tablets). The analytes were extracted with acetic acid-acetonitrile (1-99 v/v), methanol and acetone, respectively. The extract was purified using a combined column, followed by analyte detection with electrospray ionisation in positive- or negative-ion modes. The results indicated that the 30 compounds had good linear correlations in the range of 1-1000 μg kg⁻¹, and the correlation coefficients were above 0.99. The limits of detection (LOD) and limits of quantification (LOQ) were 0.03-2 and 0.1-5 μg kg⁻¹, respectively. The average recovery of 30 compounds at the three spiked levels varied from 74.7% to 124.1%, and the relative standard deviation (RSD) was 2.4-15.0%. This method was applied to the analysis of hormones in 14 real samples of which seven hormones (such as estrone, dienestrol) were detected in four samples, but the remainder of the hormones were not detected. The developed method is sensitive, efficient, reliable and applicable to real samples.

Risks and benefits related to alimentary exposure to xenoestrogens

“…For example, in recent years several emerging healthcare anti-aging products indicated to regulate blood pressure and blood glucose, contain substances, such as estradiol and 17α-ethinylestradiol, that are illegally used to improve the potency of these products (He et al, 2014). …”

Determinação de estimulantes, esteroides anabolizantes, diuréticos e laxante por HPLC-DAD e LC-MS/MS em suplementos alimentares adulterados disponíveis no Brasil

“…Mais de 95% deles foram comercializados como produtos para melhora do desempenho sexual, seguido de produtos para ganho de massa muscular e perda de peso (GILARD et al, 2015). Quanto à origem, a maior taxa de adulteração foi encontrada entre as formulações chinesas (BOGUZ et al, 2006;HE et al 2014;THEVIS et al, 2008).…”

“…(sibutramina e rimonabanto), ansiolíticos (benzodiazepínicos), antidepressivos (fluoxetina), diuréticos (bumetanida, furosemida e hidroclorotiazida), laxante (fenolftaleína), e esteroides anabolizantes (CARVALHO et al 2011;COOPMAN;CORDONNIER, 2012;CHO et al, 2014;CHO et al, 2015;HE et al, 2014;KHASAN et al 2014). Além dessas classes, substâncias hipoglicemiantes, anestésicas, hormônios para tireoide, analgésicos, dentre outros, também foram encontradas em suplementos alimentares de maneira ilícita (DECONINCK et al, 2016a;KHASAN et al, 2014;KIM et al 2014;LI et al 2010;ZHU et al 2014).…”

“…Há aproximadamente 15 anos, os esteroides anabolizantes androgênicos começaram a ser detectados em suplementos alimentares, tais quais testosterona, propionato de testosterona, DHEA, androstenediona, metiltestosterona, metasterona, metandienona, estanozolol, oxandrolona, , nandrolona, decanoato de nandrolona, trembolona decanoato de testosterona e suas concentrações encontradas estão elencadas no Quadro 4 (ABATTE et al, 2014;BOGOUZ et al, 2006;CHO et al, 2015;COOPMAN;CODORNNIER, 2012;HE, et al 2014;ODOARDI et al, 2015;PELLEGRINI et al, 2012;VAN POUCKE et al, 2007).…”

“…Diclorometano e clorofórmio também já foram reportados como solventes extratores (BOGUSZ et al, 2006;CALDAS, 2017b). Na extração sólido-líquido, após a dissolução das substâncias no solvente apropriado, essas suspensões são agitadas, imersas em banho de ultrassom, centrifugadas e filtradas (CAVALCANTE et al, 2013;HE et al, 2014;KIM et al, 2014;LIANG et al, 2006;VAN POUCK et al, 2007;THEVIS et al, 2008;VIANA et al, 2015;WOO et al, 2013;YU et al, 2010).…”