Search Results (40)

Health wines are alcoholic beverages produced by infusing traditional liquors or rice wines with natural, medicinal, and food-safe ingredients. However, to accelerate efficacy, some manufacturers illegally adulterate health wines with phosphodiesterase type 5 (PDE-5) inhibitors, which may cause severe adverse effects. This study developed a method based on ultra-high-performance liquid chromatography–time-of-flight mass spectrometry (UPLC–TOF/MS) for the rapid screening and identification of 68 PDE-5 inhibitors illegally added to health wines. After optimizing the sample preparation procedure, chromatographic conditions, mass spectrometric parameters, and primary and secondary mass spectra of the 68 PDE-5 inhibitors were acquired as reference standards. Retention times and mass spectral data were imported into the Personal Compound Database and Library, establishing a high-resolution screening database with matched drug names, molecular formulas, and accurate molecular weights. A quantitative method was validated using 11 commonly adulterated compounds, including sildenafil. The response was highly linear (r ≥ 0.9988; 0.8–400 μg/L) with low detection limits (0.2–1.0 μg/L). The average spiked recoveries were 71.2–104.1%, with relative standard deviations of ≤10.1%. Among 59 commercial health wine samples, three batches tested positive for PDE-5 inhibitors (detection rate: 5.1%). The proposed method can assist market surveillance even when reference standards are unavailable for all compounds. Full article

Cyanide, a highly toxic compound, may exist in trace amounts in distilled Chinese liquor, a traditional spirit consumed by over a billion people. To enhance the efficiency and reliability of cyanide detection, we propose a rapid, fully automated method integrating steam distillation with a continuous flow analyzer. This system combines sample pretreatment, fast distillation, and colorimetric detection using the isonicotinic-barbituric acid chromogenic system based on Lambert–Beer law (measuring at 600 nm). The standard curve exhibits an excellent linear relationship and a correlation coefficient r = 0.99959. The detection limit (0.2519 µg/L) was derived from 11 replicate blank measurements. When applied to three types of Chinese liquor, the method yields spike recovery rates ranging from 91.530% to 98.485%, and precision values between 1.177% and 1.525%. A paired t-test confirms no significant difference between this method and the national standard spectrophotometric method (t = 0.535, p = 0.615). Overall, this method offers outstanding repeatability, high accuracy, rapid analysis, and minimal manual intervention, establishing it as a reliable tool for cyanide determination and contributing to the assurance of food safety in alcoholic beverages. Full article

Selenium (Se) is an essential trace element involved in antioxidant redox regulation, thyroid hormone metabolism, and cancer prevention. Among its different forms, elemental selenium (Se⁰), particularly at the nanoscale, has gained growing attention in food, feed, and biomedical applications due to its lower toxicity and higher bioavailability compared to inorganic selenium species. However, the detection of Se⁰ in real samples remains challenging as current analytical methods are time-consuming, labour-intensive, and often unsuitable for rapid analysis. In this study, we developed a method for rapidly measuring Se⁰ using carbon nanodots (CNDs) produced from the Maillard reaction between glucose and glycine. The fabricated CNDs were water-dispersible and strongly fluorescent, with an average particle size of 3.90 ± 1.36 nm. Comprehensive characterisation by transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FTIR), fluorescence spectroscopy, and Raman spectroscopy confirmed their structural and optical properties. The CNDs were employed as fluorescent probes for the selective detection of Se⁰. The sensor showed a wide linear detection range (0–12.665 mmol L⁻¹), with a low detection limit (LOD) of 0.381 mmol L⁻¹ and a quantification limit (LOQ) of 0.465 mmol L⁻¹. Validation with spiked real samples—including ultra-pure water, tap water, and soft drinks—yielded high recoveries (98.6–108.1%) and low relative standard deviations (<3.4%). These results highlight the potential of CNDs as a simple, reliable, and environmentally friendly sensing platform for trace-level Se⁰ detection in complex food and beverage matrices. Full article

Drink spiking is a significant public safety issue, often linked to crimes such as theft and sexual assault. The detection of drugs used in these incidents is challenging due to the low concentrations (<ng) and complex matrices involved. This review explores the application of gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) to identify drugs in spiked beverages. GC-MS offers high sensitivity and specificity, and is capable of detecting drugs at ng/mL levels and distinguishing between compounds with similar structures. This review highlights the advantages of GC-MS, including its ability to simultaneously analyze multiple substances and provide detailed molecular information. Various methods for detecting gamma-hydroxybutyrate (GHB), benzodiazepines, and other drugs in beverages are discussed, emphasizing the importance of derivatization to enhance their volatility and the method’s chromatographic performance. The paper also addresses the challenges of analyzing complex beverage matrices and the need for continuous improvement in detection techniques to keep pace with the evolving drug market. Overall, GC and GC-MS are powerful tools for forensic analysis in drink spiking cases, offering reliable and accurate results, which are essential for legal and investigative processes. Full article

Background: Post-production storage plays a pivotal role in developing the characteristic flavor profile of Baijiu, a traditional alcoholic beverage in China. While aging markers remain crucial for quality authentication, the identification of reliable metabolic indicators for chronological determination requires further exploration. Methods: This study establishes a novel liquid chromatography-tandem mass spectrometry (LC-MS/MS) methodology for quantifying five linoleic acid-derived oxidative metabolites in Baijiu: 9,12,13-trihydroxy-10(E)-octadecenoic acid (9,12,13-TriHOME), 9,10-Dihydroxy-12-octadecenoic acid (9,10-DiHOME), 9-oxo-(10E,12Z)-octadecadienoic acid (9-OxoODE), 9-hydroxy-(10E,12Z)-octadecadienoic acid (9-HODE) and 13-hydroxyoctadeca-(9Z,11E)-octadecadienoic acid (13-HODE). Results: The optimized protocol demonstrated exceptional sensitivity with limits of detection at 0.4 ppb through membrane-filtered direct dilution. Calibration curves exhibited excellent linearity (R² > 0.9990) across 1.0–100.0 ppb ranges. Method validation revealed satisfactory recovery rates (87.25–119.44%) at three spiking levels (10/20/50 ppb) with precision below 6.96% RSD. Application to authentic samples showed distinct temporal accumulation patterns. Light-aroma Baijiu exhibited storage duration-dependent increases in all five oxides. Strong aroma variants demonstrated significant positive correlations for 9,12,13-TriHOME, 9,10-DiHOME, and 9-OxoODE with aging time. Conclusions: These findings systematically characterize linoleic acid oxidation products as potential aging markers, providing both methodological advancements and new insights into Baijiu aging mechanisms. Full article

In this study, Fe₃O₄ was used as a magnetic core, combined with the characteristics of mesoporous adsorbents, to prepare a novel magnetic mesoporous composite material named MMC. Cetyltrimethylammonium bromide (CTAB) and tetraethyl orthosilicate (TEOS) were used as functional monomers, and a simple etching method was employed. The resulting MMC was used as an effective adsorbent for the magnetic solid-phase extraction of trace residues of six bisphenol endocrine disruptors (bisphenol A, bisphenol B, bisphenol C, bisphenol F, bisphenol AF, and bisphenol AP) from environmental water and food samples. Characterization results indicated that the surface of MMC exhibited a distinct wormhole-like mesoporous structure, with the successful incorporation of CTAB functional groups and Si-OH. The crystal structure of Fe₃O₄ remained stable throughout the preparation process. Mapping analysis confirmed the uniform distribution of CTAB functional groups without aggregation and demonstrated high magnetic intensity, enabling rapid separation and collection under an external magnetic field. Extraction and elution conditions were optimized, and tests were conducted for interfering substances such as humic acid, glucose, fructose, and sucrose under optimal parameters. The results showed that recovery rates were not significantly affected. The quality evaluation of the method demonstrated good linearity, a broad linear range, low limits of detection and quantification, and satisfactory recovery rates. Blank and spiked analyses were conducted for seven real samples, including environmental water (rivers and lakes) and food samples (dairy, juice, and carbonated beverages), with satisfactory spiked recovery rates achieved. Thus, the developed analytical method enables the analysis and detection of trace residues of various bisphenol pollutants in complex matrices, such as environmental water and food samples, providing a valuable reference for trace analysis of similar contaminants in complex matrices. Full article

This article reports on the long-term use, solid bismuth microelectrode arrays for the first time. The presented working microelectrode is characterized by particular advantages compared to bismuth film electrodes and solid single bismuth microelectrodes; these advantages include environmentally friendly properties and the amplification of recorded currents, which are subsequently more resistant to interference. The proposed solid bismuth microelectrode array was applied to develop an adsorptive stripping voltammetric procedure for Sunset Yellow determination. The main experimental parameters were optimized. The calibration graph was linear from 5 × 10⁻⁹ to 1 × 10⁻⁷ mol L⁻¹ (time of accumulation, 60 s). The detection limit was equal to 1.7 × 10⁻⁹ mol L⁻¹. The relative standard deviation for a concentration of Sunset Yellow of 2 × 10⁻⁸ mol L⁻¹ was 4.1% (n = 7). Potential interference effects were examined. The presented analytical procedure was applied for the determination of Sunset Yellow in isotonic beverages and the results were confirmed by HPLC as a comparative method. The correctness of the presented procedure was also confirmed by satisfactory recovery values obtained during the analysis of spiked environmental water samples. Full article

Amperometric electrochemical sensing schemes, which are easily fabricated and can directly relate measured current with analyte concentrations, remain a promising strategy for the development of the portable, in situ detection of commonly employed adulterants. Xylazine (XYL) is a non-narcotic compound designed for veterinary use as a sedative known as Rompun^®. XYL is increasingly being abused as a recreational drug, as an opioid adulterant and, because of its chemical properties, has found unfortunate prominence as a date rape drug spiked into beverages. In this study, a systematic exploration and development of fouling-resistant, amperometric XYL sensors is presented. The sensing strategy features layer-by-layer (LBL) modification of glassy carbon electrodes (GCEs) with carbon nanotubes (CNTs) for sensitivity and the engagement of cyclodextrin host–guest chemistry in conjunction with polyurethane (PU) semi-permeable membranes for selectivity. The optimization of different materials and parameters during development created a greater fundamental understanding of the interfacial electrochemistry, allowing for a more informed subsequent design of effective sensors exhibiting XYL selectivity, effective sensitivity, rapid response times (<20 s), and low estimated limits of detection (~1 ppm). Most importantly, the demonstrated XYL sensors are versatile and robust, easily fabricated from common materials, and can effectively detect XYL at <10 ppm in both common alcoholic and non-alcoholic beverages, requiring only minimal volume (20 µL) of the spiked beverage for a standard addition analysis. Full article

In this paper, we report the possibility of using the X-ray powder diffraction (XRPD) technique to detect gamma-hydroxybutyric acid (GHB) in the form of its sodium salt in different beverages, but because it is not possible to freely buy GHB, beta-hydroxybutyric acid (BHB) and its sodium salt (NaBHB) were used as a model to fine-tune an X-ray diffraction method for the qualitative analysis of the sodium salt of GHB. The method requires only a small quantity of beverage and an easy sample preparation that consists only of the addition of NaOH to the drink and a subsequent drying step. The dry residue obtained can be easily analyzed with XRPD using a single-crystal X-ray diffractometer, which exploits its high sensitivity and allows for very fast pattern collection. Several beverages with different NaBHB:NaOH molar ratios were tested, and the results showed that NaBHB was detected in all drinks analyzed when the NaBHB:NaOH molar ratio was 1:50, using a characteristic peak at very low 2θ values, which also permitted the detection of its presence in complex beverage matrices. Moreover, depending on the amount of NaOH added, shifting and/or splitting of the characteristic NaBHB salt peak was observed, and the origin of this behavior was investigated. Full article

Barley, an ancient crop, was vital for early civilizations and has historically been served as food and beverage. Today, it plays a major role as feed for livestock. Breeding modern barley varieties for high yield and quality has created significant genetic erosion. This highlights the importance of tapping into genetic and genomic resources to develop new improved varieties that can overcome agricultural bottlenecks and increase barley yield. In the current study, 75 barley genotypes were evaluated for agro-morphological traits. The relationships among these traits were determined based on genotype by trait (GT) biplot analysis for two cropping years (2021 and 2022). This study was designed as a randomized complete block experiment with four replications. The variation among genotypes was found to be significant for all traits. The correlation coefficient and GT biplot revealed that grain yield (GY) was positively correlated with the number of grains per spike (NGS), the grain weight per spike (GW), and the thousand kernel weight (1000 KW). However, the test weight (TW) was negatively correlated with the heading date (HD). Hierarchical analysis produced five groups in the first year, four groups in the second year, and four groups over the average of two years. Genotypes by trait biplot analysis highlighted G25, G28, G61, G73, and G74 as promising high-yielding barley genotypes. This study demonstrated the effectiveness of the GT biplot as a valuable approach for identifying superior genotypes with contrasting traits. It is considered that this approach could be used to evaluate the barley genetic material in breeding programs. Full article

A liquid–liquid extraction pretreatment method using n-hexane as the extractant was developed for the analysis of volatile aroma substances in three flavors (six cola samples, six lemon samples, and six orange samples) of carbonated beverages by gas chromatography–mass spectrometry (GC-MS). Quantitative analysis was conducted using the external standard method. The spiked recovery rate of α-terpineol was used as the evaluation criterion. Single-factor and response surface experiments were conducted to investigate the effects of extraction temperature, extraction time, and solvent-to-sample ratio. The results indicated that the maximum spiked recovery rate of α-terpineol, 81.00%, was achieved at an extraction temperature of 45 °C, extraction time of 30 min, and a solvent-to-sample ratio of 1 mL:15 mL. Thirty-four components were identified by GC-MS on the pretreated samples via the internal standard method. 1,4-Cineole, fenchyl alcohol, borneol, and α-terpineol are covered aroma substances in cola beverages. Two aromatic substances, D-limonene and α-terpineol, were detected in orange juices. α-Terpineol was detected in each lemon-flavor carbonated beverage sample. Going a step further, α-terpineol was detected in all 18 carbonated beverage samples and had high response values. The principal component analysis by functional group classification led to the conclusion that acids, phenols, hydrocarbons, alcohols, and ethers played a major contribution to the aroma of these 18 beverages. Increased separation of target compounds was found using the new pre-treatment methods, resulting in improved analytical resolution and selectivity. Full article

Post-fermented tea (PFT) is one of the most commonly consumed beverages worldwide. Rapid microbial growth and significant changes in the microbial composition of PFT during processing and storage pose a potential risk of contamination with mycotoxins such as zearalenone (ZEN). Screening for ZEN contamination in a simple, rapid, and inexpensive manner is required to ensure that PFT is safe for consumption. To monitor ZEN in PFT, ZEN was conjugated with bovine serum albumin to prepare egg yolk immunoglobulins (IgY). A specific indirect competitive enzyme-linked immunosorbent assay (ic-ELISA) based on IgY was developed and validated. ZEN was extracted with acetonitrile and water (50:50, v/v) containing 5% acetic acid and purified using a mixture of primary and secondary amines and graphitized carbon black to remove matrix interference from the PFT samples. Under optimal conditions, the linear range of this assay was 13.8−508.9 ng mL⁻¹, the limit of detection was 9.3 ng mL⁻¹, and the half-maximal inhibitory concentration was 83.8 ng mL⁻¹. Cross-reactivity was negligible, and the assay was specific for ZEN-related molecules. The recovery rate of ZEN in the control blanks of PFT samples spiked with a defined concentration of ZEN of 89.5% to 98.0%. The recovery and accuracy of the method were qualified for PFT matrices. No significant differences were evident between the results of the actual PFT samples analyzed by high-performance liquid chromatography and ic-ELISA. The collective data indicate that the developed ic-ELISA can be used for the rapid and simple detection of ZEN in PFT products. Full article

Illicit drug misuse has become a widespread issue that requires continuous drug monitoring and diagnosis. Wearable electrochemical drug detection devices possess the potential to function as potent screening instruments in the possession of law enforcement personnel, aiding in the fight against drug trafficking and facilitating forensic investigations conducted on site. These wearable sensors are promising alternatives to traditional detection methods. In this study, we present a novel wearable electrochemical glove-based analytical device (eGAD) designed especially for detecting the club drug, methamphetamine. To develop this sensor, we immobilized meth aptamer onto silver nanoparticle (AgNPs)-modified electrodes that were printed onto latex gloves. The characteristics of AgNPs, including their shape, size and purity were analysed using FTIR, SEM and UV vis spectrometry, confirming the successful synthesis. The developed sensor shows a 0.1 µg/mL limit of detection and 0.3 µg/mL limit of quantification with a linear concentration range of about 0.01–5 µg/mL and recovery percentages of approximately 102 and 103%, respectively. To demonstrate its applicability, we tested the developed wearable sensor by spiking various alcoholic and non-alcoholic drink samples. We found that the sensor remains effective for 60 days, making it a practical option with a reasonable shelf-life. The developed sensor offers several advantages, including its affordability, ease of handling and high sensitivity and selectivity. Its portable nature makes it an ideal tool for rapid detection of METH in beverages too. Full article

We present the development of an electrochemical paper-based analytical device (ePAD) for the detection of methamphetamine. Methamphetamine is a stimulant that young people use as an addictive narcotic, and it must be detected quickly since it may be hazardous. The suggested ePAD has the advantages of being simple, affordable, and recyclable. This ePAD was developed by immobilizing a methamphetamine-binding aptamer onto Ag-ZnO nanocomposite electrodes. The Ag-ZnO nanocomposites were synthesized via a chemical method and were further characterized via scanning electron microscopy, Fourier transform infrared spectroscopy, and UV-vis spectrometry in terms of their size, shape, and colloidal activity. The developed sensor showed a limit of detection of about 0.1 μg/mL, with an optimum response time of about 25 s, and its extensive linear range was between 0.01 and 6 μg/mL. The application of the sensor was recognized by spiking different beverages with methamphetamine. The developed sensor has a shelf life of about 30 days. This cost-effective and portable platform might prove to be highly successful in forensic diagnostic applications and will benefit those who cannot afford expensive medical tests. Full article

In recent years, several innovative food processing technologies such as ultrasound (USN) and pulsed electric fields (PEF) have emerged in the market, showing a great potential both alone and in combination for the preservation of fresh and processed products. Recently, these technologies have also shown promising applications to reduce mycotoxin levels in food products. Therefore, the objective of this study is to investigate the potential of the combined treatments USN + PEF and PEF + USN on the reduction of Ochratoxin A (OTA) and Enniatins (ENNs) of an orange juice mixed with milk beverage. For this purpose, the beverages were elaborated in the laboratory and individually spiked with mycotoxins at a concentration of 100 µg/L. They were then treated by PEF (30 kV, 500 kJ/Kg) and USN (20 kHz, 100 W, at a maximum power for 30 min). Finally, mycotoxins were extracted using dispersive liquid-liquid microextraction (DLLME), and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS-IT) was employed to determine them. The results showed promising applications, with reductions up to 50% for OTA and up to 47% for Enniatin B (ENNB) after the PEF + USN treatment combination. Lower reduction rates, up to 37%, were obtained with the USN + PEF combination. In conclusion, the combination of USN and PEF technologies could be a useful tool to reduce mycotoxins in fruit juices mixed with milk. Full article