Journal of chromatography open最新文献

Phytosterols (PSs) are bioactive compounds in the sterol family, present in numerous complex food and plant matrices in free and conjugated forms. The interest in these compounds arises for phytotherapeutic purposes, particularly for their action on cholesterol metabolism and impact on cardiovascular diseases. There is a need to develop approaches that can selectively extract target analytes and accurately identify and quantify them with high precision. This work proposed the synthesis of molecularly imprinted polymers (MIPs) for PSs with a sonochemical approach, enabling a rapid polymerization step (5 min). This proposed MIP was able to extract 8 PSs (brassicasterol, stigmastanol, campesterol, campestanol, stigmasterol, β-sitosterol, Δ⁵-avenasterol, α-spinasterol) from a wide range of plant and food matrices belonging to different classes (Brassicaceae, dried fruits and Leguminosae) and was coupled to ultra-high liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). MIP based on dispersed solid phase extraction (dSPE-MIP) and targeted analysis has proven to be particularly effective in addressing the challenges associated with the complexity of plant-derived matrices, minimising interferences. This was demonstrated by the excellent control of the matrix effect, which was within ±15 %, ensuring the robustness and reliability of the method. The identification and quantification of 8 different PSs was successfully achieved with satisfactory recovery values ranging from 65 % to 100 %. The proposed strategy offers an affordable alternative to classical methods, providing enhanced sensitivity, selectivity and overall performance.

The slow formation and renewal of soil, coupled with the multitude of services it provides to humanity, render this resource a critical component of the biosphere. The maintenance of soil structure and the accumulation of carbon, as well as the maintenance of biodiversity in soils, rely on the contribution of different fractions of soil organic matter. Despite its minor component in soils, the lipid fraction is of particular importance. Its functional diversity offers an inherent diagnostic value regarding soil organic matter, microbial biodiversity and the pedological processes to which the soil is subjected. Soil lipids are comprised of diverse groups of organic compounds, exhibiting structural variations from derivatives of complex organic components (e.g., phosphoglycerides or phospholipids, sphingomyelins, glycosphingolipids) to simpler functional classes which can combine to form other compounds such as wax esters, acylglycerols, sterols, terpenoids, and fatty acids. The analytical strategy for determining lipids in soils commonly involves extracting the lipids, then fractionating, hydrolyzing, derivatizating, identifying, and/or measuring them by chromatography. These sample treatment procedures for lipid analysis in this complex matrix are typically traditional. While sustainable sample preparation procedures are not yet fully implemented, the analysis of intact lipids by liquid chromatography coupled to mass spectrometry detection is becoming more common to avoid fractionation and derivatization. This paper reviews current sample preparation strategies for the analysis of soil lipids and presents some alternatives to the traditional methods used for soil lipid extraction, fractionation, and derivatization.

The separation and analysis of chiral compounds is an important topic in various fields such as research, pharmaceutical industry, food control, agrochemistry, biochemistry, forensics and toxicology, etc. The interest in the mentioned fields is mainly due to the fact that enantiomers could react with the chiral environment. Therefore, their separation and analysis are a challenging issue because the use of these compounds can be related to humans and animals’ lives as well as to the environment (e.g., soil and water). Their separation can be performed with different analytical techniques such as high-performance liquid chromatography, gas chromatography, supercritical fluid chromatography, and microfluidic technique (capillary electrophoresis and capillary electrochromatography-CEC). Usually the direct resolution method is applied making use of a chiral stationary phase (CSP). This tutorial is aimed at illustrating the main features of CEC using a packed capillary, e.g., employing a silica-vancomycin CSP. The synthesis of the CSP, the instrumentation of CEC coupled with UV and mass spectrometry detectors, method optimization, and two selected applications are presented and discussed.

Food analysis plays an important role in preserving the integrity and quality of food. Despite these noble goals, most official methods for the analysis of nutrients (vitamins, carotenoids, etc.) antioxidants (polyphenols, etc.), and contaminants (pesticides, veterinary drugs, mycotoxins etc.) still rely on time-consuming, complex, and polluting procedures of sample preparation. To solve this discrepancy, the scientific community has frantically been working to make extraction procedures faster and safer, resorting to miniaturization, automation, low-energy consumption, and solvents/sorbents from renewable resources. This review provides an overview of the most sustainable extraction methods in food analysis, developed over the last ten years (2014–2024), including relevant examples of both liquid phase and sorbent-based techniques. Particular emphasis is placed on solutions aimed at improving the method sustainability such as smart devices, neoteric solvents, and composite sorbents, discussing the latest advancements and future trends in this sector.

The objective of the present study was to determine the inorganic and organic arsenic species and assess the actual risk of selected seafood produced in Sri Lanka in terms of inorganic arsenic species. A total of 80 samples, comprising 75 seafood samples and 5 freshwater samples, including mollusks, echinoderms, and crustaceans, were analyzed for their total arsenic (TA) levels and arsenic species. TA levels in seafood were determined using Inductively Coupled Plasma Mass Spectrometry (ICP-MS) after microwave digestion. Arsenic species, including arsenobetaine (AsB), arsenite (As^III), arsenate (As^V), monomethylarsonic acid (MMA), and dimethylarsinic acid (DMA), were selectively separated and quantified using High-Performance Liquid Chromatography (HPLC) coupled to ICP-MS, following water bath extraction with 30 mmol/L nitric acid. The TA levels in seafood ranged from 0.036 to 11.686 mg kg^-1. The spike recovery values for the five arsenic species lay within 80 % to 120 %, and the chromatographic recovery percentages ranged from 85.5 % to 123.6 %. In most samples, 100 % AsB was detected. Sea cucumber and both marine and freshwater giant river prawns showed AsB percentages of the total arsenicals at 83.2 %, 39.7 %, and 21.3 %, respectively. DMA was found in sea cucumber and marine giant river prawn at levels of 0.065 mg kg^-1 and 0.048 mg kg^-1, respectively, while MMA was not detected in any samples. As^III was found in marine water giant river prawn and freshwater giant river prawn at levels of 0.010 mg kg^-1 and 0.044 mg kg^-1, respectively. As^V was only found in marine giant river prawn at a concentration of 0.193 mg kg^-1. No other samples contained detectable levels of inorganic arsenicals. The Target Hazard Quotient (THQ) values for marine and freshwater giant river prawn were 0.90 and 0.2, respectively, indicating no significant health risks since the THQ values were <1. Therefore, our study suggests that consuming the studied seafood does not pose any health risks in terms of arsenic.

The review compiles a selection of the recently published chemical research on stilbenes, stilbene glucuronides, and stilbenoids. The basic structure of stilbene group compounds is 1,2-diphenylethene. They can be isolated from spruce, pine, and other conifers, and specifically from wood bark, needles, heartwood, and roots.

Stilbenes and stilbenoids possess antioxidative, anti-inflammatory, and antimicrobial impacts what for they are used in pharmaceuticals. They decrease of glucose and triglyceride concentrations in plasma. Especially, they are used for treatment of cancer, liver injuries, and Alzheimer's disease.

Lately, extraction of stilbene group compounds from wood materials was done with alcohol, water, or nonpolar solvents. Moreover, they were extracted with supercritical fluid and hot water extraction methods. Rectified extracts were studied with liquid and/or gas chromatography. Mass spectrometry with negative electrospray ionization was the prevalent method for their identification. HPLC-MS methods were preferred over GC to identify dimeric stilbenes and oligomeric stilbenoids.

Edible flowers have been consumed from ancient times and it was believed to deliver medicinal properties. This study explored some common edible flowers from Assam, India, such as Night Jasmine (Nyctanthus arbortristis), Drumstick (Moringa oleifera), Pumpkin (Cucurbita spp.), and Nongmangkha (Phlogacanthus thyrsiflorus), to assess their nutritional values, phytochemical characteristics, antioxidant potential, and mineral content. Additionally, the study aimed to analyze the presence of various phenolic compounds in these flowers using HPLC. Nongmangkha flowers exhibited the highest total phenolic content (TPC) of 118.12 mg GAE/g and total flavonoid content (TFC) of 75.36 mg QE/g. Drumstick flowers showed the highest ash content at 6.55 % and also the highest DPPH radical scavenging activity at 89.76 %. Potassium was found among all these flowers ranged from 11.95 to 4.412 mg/g, zinc 0.046 to 0.130 mg/g and iron 0.235 to 0.513 mg/g. HPLC screening showed that, Night jasmine flowers had gallic acid, resorcinol, caffeic acid, p-coumeric acid, ferulic acid. The findings of this study are valuable for understanding the nutritional composition of these edible flowers. Additionally, further scientific research is needed on their bioaccessibility and bioavailability, as well as on the application of these flowers in the development of food products

This review is aimed at providing an overview of the application of liquid chromatography-high resolution mass spectrometry (LC-HRMS) in the metabolomic study of cereal grains, with special emphasis on wheat, maize, barley, and rice. The significant role of untargeted metabolomics in identifying and quantifying metabolites is highlighted, thereby elucidating biochemical pathways involved in flavour, disease detection, and the development of disease-resistant varieties. The use of stable isotope labelling for enhanced compound annotation and the exploration of metabolic pathways involved in plant defence mechanisms and stress resilience are also discussed. The integration of cutting-edge analytical techniques is becoming of fundamental importance to enhance the understanding of metabolic reconfigurations in response to various conditions, thereby contributing to the improvement of cereal quality and ensuring food safety. The potential health benefits of phytochemicals in human nutrition and the role of specific metabolites as biomarkers for crop resistance and susceptibility to diseases, pests, and abiotic stresses are discussed. Overall, valuable insights into the advancement of analytical chemistry and its applications in agricultural science are provided by this review.

This study investigated the physicochemical and antioxidant properties of stingless bee (Tetragonula carbonaria) cerumen from Australia, while also identifying some phenolic constituents using High-Performance Thin-Layer Chromatography (HPTLC). The antioxidant activity of the ethanolic T. carbonaria cerumen extracts was determined using a Ferric Reducing Antioxidant Power (FRAP) assay and a HPTLC-DPPH approach was used to identify the constituents that contribute to the antioxidant activity of the cerumen samples. For the determination of the total phenolic content (TPC), a modified Folin-Ciocalteu assay was carried out. The FRAP values ranged from 5.19 ± 0.40 to 16.2 ± 0.70 mmol Fe²⁺/kg of raw cerumen and the TPC values from 3.77 ± 0.12 to 81.3 ± 2.04 mg GAE/g of raw cerumen. The HPTLC analysis revealed the presence of gallic acid and kaempferol in the ethanolic T. carbonaria cerumen extracts which contribute to the antioxidant activity of the samples. The findings of the study demonstrate the antioxidant activity of Australian T. carbonaria cerumen and highlight the importance of more research into its chemical composition, bioactivity and potential therapeutical use.

A new derivatization reagent, phthalylglycyl chloride (PG-Cl), for the analysis of urinary amino acids was demonstrated using reversed-phase ultra-high performance liquid chromatography coupled to electrospray ionization-quadrupole-time-of-flight mass spectrometer. The study compares the limits of detection and quantification for different sample preparation techniques with the commonly used and effective method of derivatization using dansyl chloride. The stability of the derivatives was investigated, and the study includes an example of urinary amino acid analysis using PG-Cl derivatization. The optimal values for pH, temperature, and concentration of the derivatization reagent were established. Limits of quantification in the range of 0.5–500 µg/mL were obtained for different amino acids. The possibility of phthalylglycyl chloride usage for non-target screening applications and targeted analysis of amino acids in urine was discussed. An advantages and issues of PG-Cl in comparison with commonly used acyl-chlorides (FMOC-Cl and DNS-Cl) provided and discussed.