Adulterated dietary supplements commercialized in Brazil: development of a screening method and a preliminary study of cytotoxicity.

The high consumption of dietary supplements was a fundamental driver for the creation of the regulatory framework by the Brazilian governmental authorities. However, the regulatory agencies lack official low-cost methodologies to evaluate the quality of food supplements. A preliminary screening method by HPLC-DAD was proposed and validated for screening and quantification of adulterants in dietary supplements.

Regulatory framework for dietary supplements and the public health challenge.

Objective: The new regulatory framework for dietary supplements in Brazil prompted this analysis of the current outlook of these products and the challenges posed by the new guidelines.

Methods: We conducted a qualitative, observational and descriptive study of dietary supplements commercialized in Brazilian online stores with the help of the Google® search tool. We considered the ingredients on the labels, the effects attributed to these products and the commercial claims used as a means of promoting them to assess the necessary changes for the legal framework in the new guidelines.

A new approach to ion exchange chromatography with conductivity detection for adulterants investigation in dietary supplements.

The extent of adulteration of dietary supplements has significantly increased in recent years. This situation worries health authorities and requires auxiliary analytical tools for the investigation of illegal substances purposely added. Ion exchange chromatography with conductivity detection is a consolidated analytical technique for the determination of inorganic compounds in various matrices.

An Ultra-High Performance Liquid Chromatography-Electrospray Tandem Mass Spectrometric Method for Screening and Simultaneous Determination of Anorexic, Anxiolytic, Antidepressant, Diuretic, Laxative and Stimulant Drugs in Dietary Supplements Marketed for Weight Loss.

The consumption of dietary supplements is increasing every year all over the world and has been accompanied by an increased frequency of adulteration of these products with synthetic pharmaceuticals. Analytical methods that allow testing for the presence of synthetic drugs in dietary supplements are needed to detect such fraudulent practices. To investigate the adulteration of dietary supplements marketed for weight loss using different commercial appeals, we developed an analytical method using ultra-high-performance liquid chromatography-electrospray tandem mass spectrometry (UHPLC-ESI-MS/MS) for simultaneous determination of 32 drugs, including anorexics, anxiolytics, antidepressants, diuretics, laxatives and stimulants.

High-resolution continuum source graphite furnace atomic absorption spectrometry for screening elemental impurities in drugs to adhere to the new international guidelines.

New guidelines for the limits of elemental impurities in drug products were introduced by the International Council for Harmonization in 2014. While the guidelines define a limit for each element, the complete quantification of the 24 elements included is, in fact, unnecessary. An accurate "pass/fail" test to determine whether the threshold was exceeded or not could be valuable in this context.

Simultaneous determination of iron and nickel as contaminants in multimineral and multivitamin supplements by solid sampling HR-CS GF AAS.

A methodology to assay simultaneously iron and nickel present as contaminants in multimineral and multivitamin supplements was investigated. High-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis were used. Measurements were done with the secondary lines of Fe (352.

Detection and determination of undeclared synthetic caffeine in weight loss formulations using HPLC-DAD and UHPLC-MS/MS.

Caffeine is present in products marketed for weight loss, with the purpose of increasing thermogenesis and lipid metabolism. The dosage declared by the product manufacturer, or even its presence, is not always correctly described on the label. This work aimed to investigate the undeclared synthetic caffeine in weight loss formulations by a high-performance liquid chromatography with diode array detection (HPLC-DAD) method.

Extraction/Leaching of Metal-Containing Additives from Polyvinyl Chloride, Ethyl Vinyl Acetate, and Polypropylene Bags and Infusion Sets into Infusion Solutions.

Flexible medical devices are primarily made of plasticized polyvinyl chloride (PVC). In recent times, to avoid undesired migration of the PVC plasticizers, ethyl vinyl acetate (EVA) and polypropylene (PP) has replaced PVC. Nevertheless, other additives are necessary to generate useful polymeric materials.

Newborn Exposure to Polycyclic Aromatic Hydrocarbons Through Parenteral Nutrition.

Background And Objectives: Parenteral nutrition (PN) administered to newborns (NB) may be contaminated with polycyclic aromatic hydrocarbons (PAHs) and may therefore increase the contact with these toxicants in very early life stages. The aim of the study is to determine to what extent, if any, commercial products for PN are contaminated with PAHs and to determine whether these contaminants, when present in the bag content, are delivered to NB and whether 1-hydroxypyrene (1-HP), the pyrene metabolite, can be detected in the urine of exposed NB.

Methods: Commercial products and the bags administered to 10 NB during their period in the NICU were analyzed for the 16 priority US Environmental Protection Agency PAHs.

Persea americana Mill. crude extract exhibits antinociceptive effect on UVB radiation-induced skin injury in mice.

Persea americana, popularly known as avocado, has been empirically used as analgesic and anti-inflammatory including in the skin disorder treatment. Species of the genus Persea also show a photoprotective effect against UVB radiation. We investigated the antinociceptive and anti-inflammatory effects from a topical formulation containing the P.

A rapid method for identification and quantification of prostaglandins in cerebral tissues by UHPLC-ESI-MS/MS for the lipidomic in vivo studies.

An analytical method utilizing liquid chromatography coupled to mass spectrometry with electrospray ionization has been developed for the identification of prostaglandins (PGs) in cerebral tissues. The five compounds identified (thromboxane B2, prostaglandin E2, prostaglandin D2, 6-keto-prostaglandin F1 alpha and prostaglandin F2 alpha) are cellular mediators of inflammation and are involved in a variety of physiological and pathological processes by acting on membrane receptors on the surfaces of target cells. The parameters of the electrospray ionization interface were optimized to obtain the highest possible sensitivity for all compounds studied.

Determination of Polycyclic Aromatic Hydrocarbons in Commercial Parenteral Formulations and Medications Using High-Performance Liquid Chromatography with Diode Array Detection.

HPLC coupled to UV diode array detection (DAD) is proposed for the determination of polycyclic aromatic hydrocarbons (PAHs) in pharmaceutical products for parenteral administration. Because rubber is a possible source of PAHs for these products, samples stored in containers with rubber parts were selected for the analysis. The basis for method optimization was EPA Method 8310, which determines 16 priority PAHs in ground water and wastewater by HPLC using both UV and fluorescence detection.

Determination of Polycyclic Aromatic Hydrocarbons in Commercial Parenteral Formulations and Medications Using High-Performance Liquid Chromatography with Diode Array Detection.

HPLC coupled to UV diode array detection (DAD) is proposed for the determination of polycyclic aromatic hydrocarbons (PAHs) in pharmaceutical products for parenteral administration. Because rubber is a possible source of PAHs for these products, samples stored in containers with rubber parts were selected for the analysis. The basis for method optimization was EPA Method 8310, which determines 16 priority PAHs in ground water and wastewater by HPLC using both UV and fluorescence detection.

Evaluation of acute and subacute toxicity of hydroethanolic extract of Dolichandra unguis-cati L. leaves in rats.

Ethnopharmacological Relevance: Dolichandra unguis-cati L. is a native climbing plant of Brazil, popularly known as "unha de gato". It has been traditionally used mainly as an antipyretic, anti-inflammatory and anti-tumor agent, yet little toxicological information is found in the literature.

A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (LC-APPI-MS/MS) method for the determination of triterpenoids in medicinal plant extracts.

An analytical method using liquid chromatography-atmospheric pressure photoionization tandem mass spectrometry with toluene as a dopant was developed for the determination of triterpenes in medicinal plant extracts. The 12 compounds determined have been shown to exhibit biological activity, such as gastroprotective, hepatoprotective, anti-inflammatory, antiviral and anti-tumor effects. The parameters of the atmospheric pressure photoionization interface were optimized to obtain the highest possible sensitivity for all of the compounds.

Determination of Antimony in Pharmaceutical Formulations and Beverages Using High-Resolution Continuum-Source Graphite Furnace Atomic Absorption Spectrometry.

A sensitive and accurate method, employing high-resolution continuum source atomic absorption spectrometry, for the determination of antimony (Sb) was developed. Conditions such as pyrolysis and atomization temperatures, the use of chemical modifiers, and sample pretreatment were optimized for the determination of Sb in pharmaceutical preparations and beverages stored in polyethylene terephthalate (PET) containers. In addition to container analysis, the influence of time of contact, temperature, and content composition on the migration of Sb was investigated.

Vitis vinifera L. cv Pinot noir pomace and lees as potential sources of bioactive compounds.

Food and agricultural industries generate substantial quantities of phenolic-rich by-products that could be valuable natural sources of antioxidants. The aim of this study was to identify and quantify the phenolic compounds and radical scavenging activities of two by-products (pomace and lees) from Vitis vinifera L. cv Pinot noir.

Presence of Polycyclic Aromatic Hydrocarbons in Rubber Packaging Materials and in Parenteral Formulations Stored in Bottles With Rubber Stoppers.

Background: Rubber closures are the primary packaging material for sterile preparations intended for repeated use. Important features of rubber closures are achieved after additives are added to the elastomeric material that compounds the rubber. Among these additives is carbon black.

Simultaneous determination of cobalt and nickel in vitamin B12 samples using high-resolution continuum source atomic absorption spectrometry.

Nickel and cobalt were simultaneously assayed in vitamin B12 formulations by using atomic spectrometry. The proposed method is based on a compromise between the proximity of specific Ni and Co spectral lines and the relative abundances of the analytes in the samples. The analytes were found in concentrations ranging from 9.

Liquid chromatographic determination of caffeine and adrenergic stimulants in food supplements sold in Brazilian e-commerce for weight loss and physical fitness.

Methyl-xanthines and adrenergic stimulants, such as caffeine and synephrine, are commonly added to food supplements due to their stimulating and thermogenic effects. In addition, the abusive consumption of food supplements with ergogenic and aesthetic purposes has been observed worldwide. This work describes the study of caffeine, p-synephrine, hordenine, octopamine, tyramine, ephedrine and salicin as stimulants in dietary supplements marketed in Brazil for weight loss and physical fitness claims.

Ultrasound-Assisted Extraction and Biological Activities of Extracts of var. .

In this work, the antioxidant and antimicrobial activities of var. extracts obtained through ultrasound-assisted extraction are evaluated. The extracts obtained using the best extraction conditions were subjected to different hydrolysis conditions before their use in the biological tests.

Seleno- and telluro-xylofuranosides attenuate Mn-induced toxicity in C. elegans via the DAF-16/FOXO pathway.

Organochalcogens are promising pharmacological agents that possess significant biological activities. Nevertheless, because of the complexity of mammalian models, it has been difficult to determine the molecular pathways and specific proteins that are modulated in response to treatments with these compounds. The nematode worm Caenorhabditis elegans is an alternative experimental model that affords easy genetic manipulations, green fluorescent protein tagging and in vivo live analysis of toxicity.

Supercritical CO2 extraction, chemical characterisation and antioxidant potential of Brassica oleracea var capitata against HO·, O2(·-) and ROO·.

In this work were extracted bioactive compounds from Brassica oleracea var capitata using supercritical CO2 and evaluated the antioxidant potential of the extracts. Five extractions were accomplished to investigate the influence of pressure (10-25 MPa) and temperature (20-60 °C) in the extraction yield, chemical composition and antioxidant potential towards peroxyl, superoxide and hydroxyl radicals. The highest extraction yield was obtained at 60 °C and 25 MPa, which was 0.

Determination of diuretics and laxatives as adulterants in herbal formulations for weight loss.

A new method is described for the determination of the most common diuretic and laxative adulterants found in formulations of anorexics and antidepressants. The method is based on the separation of furosemide, hydrochlorothiazide, chlorthalidone and amiloride (diuretics), phenolphthalein (laxative), amfepramone (anorexic) and fluoxetine and paroxetine (antidepressants) by capillary zone electrophoresis with capacitively coupled contactless conductivity detection. The method showed a precision ranging from 1.

High-performance liquid chromatographic analysis of biogenic amines in pharmaceutical products containing Citrus aurantium.

A reverse-phase (RP)-HPLC method is reported for determining L-tyrosine, p-octopamine, synephrine, tyramine and hordenine as chemical markers of the species Citrus aurantium in raw material, dry extracts and phytotherapeutic herbal formulations. Using RP-HPLC with diode array detection (DAD) and gradient elution, the amines were determined in 12 different products from different Brazilian states labelled as containing C. aurantium.