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[Display omitted] • Exploration of anticancer dipeptide Aurantiamide acetate from the seeds of Brassica species. • Traditional 'Kolhu' method showed remarkable efficiency in extracting dipeptides. • Phytometabolite profiling was done by a validated UPLC-MS/QToF analytical method. • This novel method was found to be robust for the effective quantitation of dipeptides. Mustard (Brassica spp.) is one of the world's oldest condiments in the food basket, which holds a significant place in the global culinary landscape due to historical prominence and perceived health benefits. This study explores the extraction of oils from Mustard seeds by employing traditional 'Kolhu' method, modern supercritical fluid, and solvent extraction techniques. This study, for the first-time, identified Aurantiamide acetate, a potent anti-cancer dipeptide in Mustard seeds using ultra-performance liquid chromatography-mass spectrometry coupled with quadrupole time-of-flight (UPLC/MS-QToF) analytical platform. The analytical methodology was meticulously validated encompassing optimal parameters such as limit of detection, limit of quantification, precision, accuracy, linearity and robustness, within the range. Interestingly, 'Kolhu' method of oil extraction exhibited better yield of Aurantiamide acetate, suggesting superior efficiency of traditional methods. This study accentuates the importance of classical extraction methods, used traditionally, and emphasizes that naturally occurring substances indeed could be harnessed for better health. [ABSTRACT FROM AUTHOR]

New methods for the analysis of azithromycin (AZM) have been devised, employing direct fluorescence and spectrophotometric techniques. This research focused on the development and validation of these methods, especially based on the formation of an ion-pair complex with fluorescein isothiocyanate (FITC). The resulting complex enhanced the fluorescence intensity at a wavelength of 520 nm and the absorbance at 480 nm. The impact of different solvent compositions was investigated, with methanol and a 1:1 mixture of methanol and Milli-Q proving to be the most sensitive. The optimal FITC concentration was determined as 50 µg/ml, and the molar ratio of the AZM-FITC ion-pair complex was determined to be 1:1. Notably, an instantaneous increase in fluorescence intensity was observed, eliminating the need for incubation. The developed methods were validated for sensitivity, accuracy, and precision, with the fluorescence-based method demonstrating superior sensitivity and precision compared to the spectrophotometric method. Under optimum conditions, the fluorescence-based method achieved a linear range of 0–31.25 µg/ml with a limit of detection (LOD) of 0.41 µg/ml and a limit of quantification (LOQ) of 1.23 µg/ml., In contrast, the spectrophotometric method had an LOD of 0.82 µg/ml and an LOQ of 2.49 µg/ml. Additionally, the fluorescence-based method exhibited a narrower recovery range in artificial urine samples, suggesting higher precision in complex matrices. Overall, these methods offer rapid and sensitive AZM analysis with potential applications in diverse matrices such as biological samples post-extraction. • Residual trace azithromycin elevates antimicrobial resistance. • Direct optical detection of azithromycin in urine. • Azithromycin-fluorescein isothiocyanate ion pair complex. • Fluorescence-based detection of azithromycin using fluorescein isothiocyanate. • Spectrophotometric detection of azithromycin using fluorescein isothiocyanate. [ABSTRACT FROM AUTHOR]

In the pharmaceutical industry, the unexpected appearance of crystalline forms could impact the therapeutic efficacy of an Active Pharmaceutical Ingredient (API). For quality control, a thorough qualitative and quantitative monitoring of pharmaceutical solid forms is essential to ensure the detection and the quantification of crystalline forms, wither different or with the same chemical composition (polymorphs) at a low detection level. The purpose of this paper was to review and highlight the importance of choosing adequate solid-state techniques for detection and quantification APIs that present polymorphism – based on limits of detection (LOD) and quantification (LOQ), pharmacopeias specifications, international guidelines and studies reported in the literature. To this study, the powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), Infrared and Raman spectroscopies and solid-state nuclear magnetic resonance (NMR) were the solid-state techniques analyzed. Additionally, the Argentine, Brazilian, British, European, International, Japanese, Mexican and the United States of America pharmacopeias were reviewed. Based on the analysis performed, the advantages and disadvantages of these techniques, as well as the LOD and LOQ values of APIs were reported. In comparison to these solid-state techniques, reference material used for identification analyses should be previously identified with the corresponding polymorph. Without this previous procedure, the patterns, the spectra, and DSC curves of the reference material can only be used to confirm the mixture of solid forms, not being able to specify which polymorphs are contained in the sample. A major advantage of PXRD is the use of the calculated diffraction patterns obtained from the Crystallographic Information Frameworks (CIFs) files which could be used as a reference pattern without any other information, assistance technique, or physical standards. Regarding the quantification aspect, different pharmacopeias suggest various methods such as the PXRD combining with Rietveld method, which can be used to obtain lower LOD values for minority phases in the mixture of different substances without the need for a calibration curve. Raman spectroscopy can detect polymorphs in small particles and solid-state NMR spectroscopy is a powerful technique for quantification not only crystalline but also crystalline-amorphous mixtures. Finally, this review intends to be a useful tool to control, with efficiency and accuracy, the polymorphism of APIs in pharmaceutical compounds. [Display omitted] • Critical analyses of different analytical solid-state techniques to improve quality control and monitoring polymorphs. • Limit of detection and quantification of analytical solid-state techniques. • Comparison of information provided from pharmacopeias about identification and quantification analysis of polymorphisms. • Advantages and disadvantages of different solid-state techniques used for identification and quantification analyses. [ABSTRACT FROM AUTHOR]

A rapid and portable analytical methodology has been developed for ibuprofen (IBU) quantification in commercial dosage tablets using a spectrometric smartphone-based system. The analytical methodology employs point-of-use approaches both for sample preparation and detection, demonstrating its potential utility for portable quality control of pharmaceutical products. In this work, IBU is dissolved in methanol and then treated with a Co(II) aqueous solution, forming a blue complex which is extractable by dispersive liquid-liquid microextraction. Then, the sample's absorption spectrum is directly measured by a spectrometric smartphone-based system using cartridge made of polyoxymethylene for solvent compatibility. The main experimental factors affecting the dispersive liquid-liquid microextraction of Co-IBU complex were optimized using a multivariate analysis. Under optimized conditions, a working range between 20 and 80 μg mL−1 was obtained with a correlation coefficient of 0.996 for 5 calibration points. The limit of detection and limit of quantification obtained were 4 and 12 μg mL−1, respectively. The performance of the proposed methodology was evaluated in commercial tablet dosage forms, and the results demonstrate the ability of the method to determine IBU in samples representative of those used in real-world quality control applications. Recovery values between 97% and 105% were obtained, which are comparable to those obtained via standard titrimetric methodology. [ABSTRACT FROM AUTHOR]

Seafood consumption is a major route for human exposure to environmental contaminants of emerging concern (CeCs). However, toxicological information about the presence of CeCs in seafood is still insufficient, especially considering the effect of cooking procedures on contaminant levels. This study is one among a few who evaluated the effect of steaming on the levels of different CeCs (toxic elements, PFCs, PAHs, musk fragrances and UV-filters) in commercially relevant seafood in Europe, and estimate the potential risks associated with its consumption for consumers. In most cases, an increase in contaminant levels was observed after steaming, though varying according to contaminant and seafood species (e.g. iAs, perfluorobutanoate, dibenzo(ah)anthracene in Mytilus edulis , HHCB-Lactone in Solea sp., 2-Ethylhexyl salicylate in Lophius piscatorius ). Furthermore, the increase in some CeCs, like Pb, MeHg, iAs, Cd and carcinogenic PAHs, in seafood after steaming reveals that adverse health effects can never be excluded, regardless contaminants concentration. However, the risk of adverse effects can vary. The drastic changes induced by steaming suggest that the effect of cooking should be integrated in food risk assessment, as well as accounted in CeCs regulations and recommendations issued by food safety authorities, in order to avoid over/underestimation of risks for consumer health. [ABSTRACT FROM AUTHOR]

Pesticide residue analysis in olive oil presents difficulties due to the high amount of co-eluted compounds resulting in high matrix effect. Different extraction/clean-up methods including gel permeation chromatography, liquid/liquid extraction, solid-phase extraction and other extraction methods are applied to overcome these difficulties. Recent approaches such as the addition of the freezing-out step and the application of Enhanced Matrix Removal-Lipid sorbent (EMR-Lipid) are reported. Gas chromatography and liquid chromatography coupled to mass spectrometry are considered the gold standard technologies covering a wide scope of pesticides. This review recapitulates the methods most widely used for the determination of pesticide residues in vegetable oils. As a continuation of previous reviews, the work conducted is an update review of methods from 2006 in this field, evaluating their strengths and limitations. Main analytical parameters of the different extraction procedures and detection methods are discussed in terms of recoveries, robustness, limit of quantification, and matrix effect. [ABSTRACT FROM AUTHOR]

Surge in consumption of healthy and safe foods has challenged researchers to develop sensitive, precise, robust detection and quantification of food contaminants like acrylamide even if they are present in trace. Keeping this in view, a robust and sensitive analytical method was developed and validated for acrylamide quantification in a potato-based food product (potato cutlet), using LC-MSMS with positive electrospray ionization (+ESI). The method consists of adding acrylamide-d 3 (deuterium labelled acrylamide) as an internal standard, extraction by modified QuEChERS method with d-SPE clean-up. Extracts were run on a reverse phase C-18 column for analysis by liquid chromatography. The limit of detection (LOD) and limit of quantification (LOQ) were determined as 0.7 and 2.0 μg kg−1, respectively, demonstrating the sensitivity of the method for trace detection. The developed method showed excellent results in terms of recoveries (91.0–109.16%), repeatability (RSD 1.8–10.60%), reproducibility (RSD 2.3–11.24%) and robustness (RSD 1.74–4.54%). The repeatability, reproducibility and robustness respectively, show the consistency, accuracy and stability of the developed method. The deviations in ion ratio and retention time were 17.25% and −0.01 min, respectively. Compared to previous findings, the current study has achieved lower LOD and LOQ levels that reveals the higher sensitivity of this method for acrylamide quantification in potato cutlet. [Display omitted] • Robust and sensitive acrylamide quantification method development for potato cutlet. • Acrylamide quantification method has been validated according to SANTE guidelines. • Lower levels of limit of acrylamide detection and quantification have been achieved. • Developed method may be applicable for other potato-based products. [ABSTRACT FROM AUTHOR]

The applicability of qPCR in olive-oil authentication depends on the DNA obtained from the oils and the amplification primers. Therefore, four olive-specific amplification systems based on the trn L gene were designed (A-, B-, C- and D-trnL systems). The qPCR conditions, primer concentration and annealing temperature, were optimized. The systems were tested for efficiency and sensitivity to select the most suitable for olive oil authentication. The selected system (D-trnL) demonstrated specificity toward olive in contrast to other oleaginous species (canola, soybean, sunflower, maize, peanut and coconut) and showed high sensitivity in a broad linear dynamic range (LOD and LOQ: 500 ng – 0.0625 pg). This qPCR system enabled detection, with high sensitivity and specificity, of olive DNA isolated from oils processed in different ways, establishing it as an efficient method for the authentication of olive oil regardless of its category. [ABSTRACT FROM AUTHOR]

Growing world demand for gold and decreasing discovery rates of ore deposits necessitates new techniques for gold exploration. Current techniques for the detection of ppb level of gold, such as inductively coupled plasma mass spectrometry (ICP-MS) are not field-deployable. By contrast, current portable device such as X-ray fluorescence (XRF) based sensors are not sufficiently sensitive. Thus, there is growing interest in developing a new, easy-to-use and fast method for detection of low concentrations of gold at the site of an exploration drilling rig. Two optical methods, absorption and fluorescence, are examined for their suitability for low gold concentration detection. Absorption study is based on the analysis of localised surface plasmon resonance peak. For fluorescence analysis, the ability of gold nanoparticles to specifically catalyse the conversion of the non-fluorescent compound (I-BODIPY) to the fluorescent derivative (H-BODIPY) is used. For both absorption and fluorescence methods, the limit of quantification (LOQ) of gold nanoparticles (NPs) was found to be dependent on the NP size (71 ppb of 5 nm and 24.5 ppb of 50 nm NPs for absorption and 74 ppb of 5 nm and 1200 ppb of 50 nm NPs for fluorescence). The LOQ for fluorescence for 50 nm NPs measured in a suspended core optical fibre was almost twice lower than in a cuvette. The field deployment potential of these methods was also determined using a portable set up. [ABSTRACT FROM AUTHOR]

Abstract: This paper extends a recent report on a model to establish population characteristics to include censored data. The theoretical background is given. The application given in this paper is limited to left-censored data, i.e. less than values, but the principles can also be adopted for other types of censored data. The model gives robust estimates of population characteristics for datasets with complicated underlying distributions including less than values of different magnitude and less than values exceeding the values of numerical data. The extended model is illustrated with simulated datasets, data from interlaboratory studies and temporal trend data on dissolved cadmium in the Rhine river. The calculations confirm that inclusion of left-censored values in the computation of population characteristics improves assessment procedures. [Copyright &y& Elsevier]

Abstract: An internal validation of the Applied Biosystems 8-capillary 3500 Genetic Analyzer was performed using two commercial short tandem repeat (STR) multiplex kits (Identifiler and Identifiler Plus). Validation experiments to evaluate the performance of this CE consisted of a precision study, sensitivity study, genotype concordance, a two person mixture study, and signal normalization evaluation. The sensitivity study consisted of duplicate injections of amplified DNA template ranging from 1.0ng down to 0.01ng. These male samples were heterozygous at all loci. Statistical evaluation of the sensitivity data was performed to determine the statistical significance between employing a single threshold across all dye channels and opting for dye specific thresholds. [Copyright &y& Elsevier]