Food supplements (FS) are often consumed as one of the strategies to fight ageing-associated pathologies, especially in the case of oxidative stress-related diseases. Despite the popularity of FS, some concerns about their quality and safety have been raised, especially regarding the presence of contaminants. This paper reviews and discusses the occurrence of contaminants in marketed samples of FS in the last two decades, considering both scientific literature and notifications registered on RASFF portal. The most relevant classes of contaminants were included namely metals, toxins, pesticides, dioxins and PCBs, as well as pharmacologically active ingredients. Variable amounts of contaminants were reported in a significant number of commercially available FS. Although the presence of contaminants does not necessarily mean that their levels exceed the regulatory limits or that the FS intake constitutes a risk to human health, it alerts for the need to further monitor FS safety. The evaluation of the risk associated to the consumption of FS, especially in the elderly population, is particularly challenging due to the frequent exposure to multiple toxicants and to different exposure sources, as well as due to possible pre-existing diseases and respective therapeutics. Therefore, improved quality control procedures and monitoring programs should be pursued in order to avoid undesirable products and assure the safety of FS.

Contaminants: a dark side of food supplements?

Molecular imprinting technology (MIT), also known as molecular template technology, is a new technology involving material chemistry, polymer chemistry, biochemistry, and other multi-disciplinary approaches. This technology is used to realize the unique recognition ability of three-dimensional crosslinked polymers, called the molecularly imprinted polymers (MIPs). MIPs demonstrate a wide range of applicability, good plasticity, stability, and high selectivity, and their internal recognition sites can be selectively combined with template molecules to achieve selective recognition. A molecularly imprinted fluorescence sensor (MIFs) incorporates fluorescent materials (fluorescein or fluorescent nanoparticles) into a molecularly imprinted polymer synthesis system and transforms the binding sites between target molecules and molecularly imprinted materials into readable fluorescence signals. This sensor demonstrates the advantages of high sensitivity and selectivity of fluorescence detection. Molecularly imprinted materials demonstrate considerable research significance and broad application prospects. They are a research hotspot in the field of food and environment safety sensing analysis. In this study, the progress in the construction and application of MIFs was reviewed with emphasis on the preparation principle, detection methods, and molecular recognition mechanism. The applications of MIFs in food and environment safety detection in recent years were summarized, and the research trends and development prospects of MIFs were discussed.

/pdf/recent-advances-and-perspectives-of-molecularly-imprinted-33x41h6fwm.pdf

Recent Advances and Perspectives of Molecularly Imprinted Polymer-Based Fluorescent Sensors in Food and Environment Analysis

A multiresidue method for the simultaneous and rapid analysis of 360 pesticides in representative agricultural produce (brown rice, orange, spinach, and potato) was developed using a modified QuEChERS procedure combined with gas chromatography–tandem mass spectrometry (GC-MS/MS). Selected reaction monitoring transition parameters (e.g., collision energy, precursor and product ions) in MS/MS were optimized to achieve the best selectivity and sensitivity for a wide range of GC-amenable pesticides. A short (20 m) microbore (0.18 mm i.d.) column resulted in better signal-to-noise ratio with reduced analysis time than a conventional narrowbore column (30 m × 0.25 mm i.d.). The priming injection dramatically increased peak areas by masking effect on a new GC liner. The limit of quantitation was 0.99 within the range of 0.0025–0.1 mg/kg. Acetonitrile with 0.1% formic acid without additional buffer salts was used for pesticide ex...

Rapid and Simultaneous Analysis of 360 Pesticides in Brown Rice, Spinach, Orange, and Potato Using Microbore GC-MS/MS

The large-scale use of pesticides such as organophosphate pesticides (OPPs) and organochlorine pesticides (OCPs) has led to serious environmental problems worldwide, and their high toxicity could cause serious damage to human health. It is crucial to remove and track them precisely in the environment and food resources. As novel nanomaterials, metal-organic frameworks (MOFs) have attracted significant attention in the fields of adsorption and luminescence sensing due to their rich topology, tunable pore size and shape, high surface area, and abundant active sites. Luminescent metal-organic frameworks (LMOFs) have sprung up as great potential chemical sensors to detect pesticides with fast response, high sensitivity, high selectivity and easy operation. Therefore, in this highlight, we focus on recent progress of MOFs in sensing and adsorbing pesticides, as well as in the possible mechanism of sensing, so as to attract more attention to pesticide detection and adsorption.

Recent advances in metal-organic frameworks for pesticide detection and adsorption.

Herbal-based dietary supplements have become increasingly popular. The extract from milk thistle (Silybum marianum), is often used for the treatment of liver diseases. However, serious concerns exist regarding the efficacy, composition, as well as the safety of these over-the-counter preparations. Therefore, the aim of the present study was to investigate the composition as well as chemical and biological safety of 26 milk thistle-based dietary supplements purchased from both the U.S. and Czech markets between 2016 and 2017. The study was focused on a determination of the composition of active ingredients, as well as analyses of possible contaminants including: mycotoxins, plant alkaloids, and pesticide residues, as well as the microbial purity. High-throughput analyses were performed using advanced U-HPLC-HRMS techniques. Large differences in the silymarin content were observed among individual milk thistle preparations, often in contrast with the information provided by the manufacturers. In addition, substantial inter-batch differences in silymarin content were also demonstrated. In all milk thistle preparations tested, large numbers and high concentrations of mycotoxins and several pesticides, as well as the substantial presence of microbiological contamination were detected, pointing to serious safety issues. In conclusion, our results strongly indicate the need for strict controls of the composition, chemical contaminants, as well as the microbiological purity of commercial milk thistle extracts used for the treatment of liver diseases. Poor definition of these preparations together with contamination by biologically active substances may not only account for the inconsistency of clinical observations, but also be responsible for possible herbal-based dietary supplements-induced liver injury.

/pdf/poor-chemical-and-microbiological-quality-of-the-commercial-33nrvc6mpl.pdf

Poor chemical and microbiological quality of the commercial milk thistle-based dietary supplements may account for their reported unsatisfactory and non-reproducible clinical outcomes.

A simplified sample preparation method in combination with gas chromatography–triple-quadrupole mass spectrometry (GC-MS/MS) analysis was developed and validated for the simultaneous determination of 227 pesticides in green tea, ginseng, gingko leaves, saw palmetto, spearmint, and black pepper samples. The botanical samples were hydrated with water and extracted with acetonitrile, magnesium sulfate, and sodium chloride. The acetonitrile extract was cleaned up using solid phase extraction with carbon-coated alumina/primary–secondary amine with or without C18. Recovery studies using matrix blanks fortified with pesticides at concentrations of 10, 25, 100, and 500 μg/kg resulted in average recoveries of 70–99% and relative standard deviation of 5–13% for all tested botanicals except for black pepper, for which lower recoveries of fortified pesticides were observed. Matrix-matched standard calibration curves revealed good linearity (r2 > 0.99) across a wide concentration range (1–1000 μg/L). Nine commercially...

Determination of Multiresidue Pesticides in Botanical Dietary Supplements Using Gas Chromatography-Triple-Quadrupole Mass Spectrometry (GC-MS/MS).

An HPLC method for simultaneous determination of vitamins A and D3 in fluid milk was developed and validated. Saponification and extraction conditions were studied for optimum recovery and simplicity. An RP HPLC system equipped with a C18 column and diode array detector was used for quantitation. The method was subjected to a single-laboratory validation using skim, 2% fat, and whole milk samples at concentrations of 50, 100, and 200% of the recommended fortification levels for vitamins A and D3 for Grade "A" fluid milk. The method quantitation limits for vitamins A and D3 were 0.0072 and 0.0026 μg/mL, respectively. Average recoveries between 94 and 110% and SD values ranging from 2.7 to 6.9% were obtained for both vitamins A and D3. The accuracy of the method was evaluated using a National Institute of Standards and Technology standard reference material (1849a) and proficiency test samples.

Development and validation of a high performance liquid chromatographic method for simultaneous determination of vitamins A and D3 in fluid milk products.

A proficiency test (PT) program for determination of total As in apple juice samples was conducted by the Food Emergency Response Network (FERN) laboratories. An analytical method using inductively coupled plasma (ICP)-MS was validated for this project. The LOD and LOQ were determined to be 0.315 and 2.32 ng/g, respectively. A total of eight apple juice samples were sent to 38 FERN laboratories, and results were statistically evaluated according to ISO 13528:2005. The total As concentrations in the PT samples reported by the participating laboratories were very close to those obtained in the homogeneity and stability tests. The reproducibility, repeatability, interlaboratory, and intralaboratory variability results led to 69% of participating laboratories being rated as satisfactory using the widely accepted Izl score <or= 2 criterion. The percentage of laboratories with acceptable z scores (Izl scores <or=2) increased from 61 to 89% with the increase in As concentration in PT samples from 5.05 to 30.72 ng/g. This study demonstrated that the ICP/MS method was adequate for total As determination in fruit juice, and most of the participating laboratories were proficient in their analytical performance.

Method validation and proficiency testing for determination of total arsenic in apple juice by inductively coupled plasma/ mass spectrometry.

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Determination of Multiresidue Pesticides in Botanical Dietary Supplements Using Gas Chromatography-Triple-Quadrupole Mass Spectrometry (GC-MS/MS).

Development and validation of a high performance liquid chromatographic method for simultaneous determination of vitamins A and D3 in fluid milk products.

Method validation and proficiency testing for determination of total arsenic in apple juice by inductively coupled plasma/ mass spectrometry.