Determination of adulterants in whey protein food supplements by liquid chromatography coupled to Orbitrap high resolution mass spectrometry

Abstract

Liquid chromatography coupled to Orbitrap high resolution mass spectrometry was shown to be an adequate technique to control the adulteration of whey protein food supplements with prohibited substances, not declared on the labels. An extraction method combined with an instrumental analysis that allowed for the determination of 105 substances in whey protein food supplements, was established. The pre-treatment of the samples consisted of protein precipitation and solid-phase extraction using weak cation exchange functionalized polymeric sorbent cartridges. The samples were directly analyzed by LC-Orbitrap-HRMS. The selectivity, limit of detection, repeatability, recovery, carryover and matrix effect were estimated as the validation parameters. The repeatability obtained was 96.19% and the recovery 83.80%, but carryover and the matrix effect were not observed. The present method was successfully applied to the analysis of commercial samples, verifying adulteration by diuretics (conivaptan and politiazide) and a stimulant (benfluorex) in seven of the eleven brands evaluated.

Abusive use of anabolic androgenic steroids, male sexual dysfunction and infertility: an updated review

“…Attention should also be taken to dietary supplements (e.g., in the format of powders, pills, gels, bars, shakes, and/or liquids) commercialized through different distribution channels (e.g., supermarkets, gyms, hypermarkets, nutritional and “natural products” stores, drugstores, and/or online). These supplements may contain AAS substances not listed on their label, such as: pro-androgenics, xenoestrogens, estrogens, selective androgen-receptor modulators, nonsteroidal antiestrogens, anti-hypertensives, beta blockers, beta-2-adrenergic stimulants, beta-2-receptor agonists, diuretics, vasodilators, statins, adrenaline derivatives, tocolytic drugs used to stop premature labor, selective bronchodilators and anti-asthma medications, coughing inhibitors, a wide array of amphetamines, painkillers, stimulants, appetite inhibitors, and even cocaine ( Roiffé et al, 2019 ; Hallak, 2020 ).…”

Suplementos alimentares: uma fonte de doping não intencional?

“…Com relação às substâncias não declaradas, cinco produtos avaliados apresentaram cafeína em sua constituição. Ainda no que diz respeito à análise de whey protein, em estudo realizado no Laboratório Brasileiro de Controle de Dopagem (LBCD) foram verificadas adulterações em 7 das 11 marcas de suplementos proteicos derivados do soro do leite avaliados (Roiffé et al, 2019). Quatro desses produtos continham benfluorex, um estimulante que está associado à morte de cerca de 1300 pessoas na França no período de 1976 a 2009.…”

Pre‐workout supplements marketed in Brazil: Caffeine quantification and caffeine daily intake assessment

“…Considerable labeling inconsistencies are reported in the literature with respect to the analysis of dietary supplements 19–21 . Regarding PWS, there are three major issues: the contamination with undeclared substances; the presence of stimulants that are declared on label but are not approved by the regulatory agencies; and inaccurate caffeine values 22–24 .…”

“…18 Considerable labeling inconsistencies are reported in the literature with respect to the analysis of dietary supplements. [19][20][21] Regarding PWS, there are three major issues: the contamination with undeclared substances; the presence of stimulants that are declared on label but are not approved by the regulatory agencies; and inaccurate caffeine values. [22][23][24] In fact, the inaccurately labeling problem is not specific to caffeine but rather reflects a broader problem regarding the quantity of stimulants found in PWS, including other substances, such as small components of botanicals (e.g., yohimbine and higenamine).…”