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This study quantified, for the first time, 2-isopropylmalic and 3-isopropylmalic acids, in green, roasted and espresso coffee by UHPLC-MS/MS. Moreover, it reports the influence of postharvest processing methods (natural, washed and honey) on their content. New extraction techniques were developed and validated from three coffee matrices (green, roasted and espresso). Honey coffee exhibited levels substantially higher of 2-isopropylmalic acid than those processed by natural and washed methods (p < 0.05). Specifically, 2-isopropylmalic acid levels in honey green, roasted and espresso coffee samples were 48.24 ± 7.31 ng/g, 168.8 ± 10.88 ng/g and 177.5 ± 9.49 ng/g, respectively. This research highlights the significant impact of processing methods on the chemical profile of coffee and introduces 2-isopropylmalic and 3-isopropylmalic acids as potential quality indicators. Moreover, it suggests that the fermentation stage during processing may play a crucial role in their formation, laying the foundation for optimizing coffee processing to enhance quality., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

In this study, a rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the targeted analysis of 98 New Psychoactive Substances (NPS) from the hair matrix. The monitored compounds included various chemical classes (7 phenethylamines, 10 tryptamines, 18 cathinones, 24 synthetic opioids, and 38 synthetic cannabinoids) with emphasis given to newly emerged NPS. The method employed a direct extraction process through the incubation of hair samples (25 mg) and internal standards with M3® reagent at 100 °C for 60 min, followed by extract purification through acid and basic liquid-liquid micro-extraction (LLME). Extracted compounds were analyzed through LC-MS/MS system operating in multiple reaction monitoring mode. NPS were separated in 9.5 min with a Poroshell 120 EC-C18 column (2.7 μm, 4.6 × 50 mm) using a gradient eluting mobile phase composed of water and acetonitrile/water (95:5) both containing 0.1 % of formic acid. The developed and validated method shows a good precision (≤ 15 %), linearity (R 2 between 0.993 and 0.999), selectivity, and sensitivity (LOD: 0.6-10.3 pg mg -1 and LOQ: 2.1-34.4 pg mg -1 ). The method showed also reduced matrix effect and acceptable recovery for most of the targeted compounds. Our results showed that this method is suitable for quantifying NPS in hair matrix and could be employed in the context of routine analyses in analytical laboratories., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021 Elsevier B.V. All rights reserved.)

A new fast and easy analytical procedure for the simultaneous detection and quantification of 9 anabolic steroids (deslorelin, dexamethasone sodium phosphate, prednisolone, methylprednisolone, stanozolol, boldenone, nandrolone, dexamethasone isonicotinate and altrenogest) in horse urine for doping control have been developed by using the ultra-high-performance liquid chromatography coupled with tandem mass spectrometry technique (UHPLC-MS/MS). A total amount of 400 μl of sample was evaporated, restored and injected in the UHPLC-MS/MS. The proposed method was fully validated showing a recovery higher than 89.12% and a coefficient of variation lower than 6.02%. The correlation coefficients range of the analyzed compound's calibration curves was 0.9955-0.9997, and the limits of detection and quantification were in the range of 0.1 and 0.25 μg/l, respectively., (Copyright © 2019 Elsevier B.V. All rights reserved.)

A new method for extracting isoflavones from espresso coffee (EC) was coupled with high-performance liquid chromatography-tandem mass spectrometry (MS/MS) for the first time to analyse five isoflavones, which included both a glycosilated form, genistin and the aglycons daidzein, genistein, formononetin and biochanin A. Isoflavones were extracted from coffee samples using methanol, stored in a freezer overnight to precipitate proteic or lipidic residues and purified on SPE C18 cartridges before high-performance liquid chromatography-MS/MS analysis. The recovery percentages obtained by spiking the matrix at concentrations of 10 and 100 µg l(-1) with a standard mixture of isoflavones were in the range of 70 to 104%. The limits of detection and limits of quantification were in the range of 0.015-0.3 µg l(-1) and 0.05-1 µg l(-1) , respectively. Once validated, the method was used to analyze the concentrations of isoflavones in six ECs and ten ground coffee samples. Only formononetin and biochanin A were found, and their respective concentrations ranged from 0.36 to 0.41 µg l(-1) and from 0.58 to 3.26 µg l(-1) in ECs and from 0.36 to 4.27 µg kg(-1) and from 0.71 to 3.95 µg kg(-1) in ground coffees. This method confirms the high specificity and selectivity of MS/MS systems for detecting bioactives in complex matrices such as coffee.Copyright © 2016 John Wiley & Sons, Ltd., (Copyright © 2016 John Wiley & Sons, Ltd.)

Legumes are an excellent source of macronutrients and phytochemicals as isoflavones. The aim of this work was to develop a new analytical method for determining five isoflavone compounds, three of which are aglycons, namely daidzein, genistein, biochanin A, and two of which, daidzin and genistin, are glycosilated, in lentils and other pulses, using an effective clean-up system and UHPLC-MS/MS (triple quadrupole) method. The recoveries obtained by spiking the lentil samples with a standard mixture of isoflavones at three levels of fortification (5, 25 and 100 μg kg(-1)) were in the range of 54.4-111.1%, 68.6-91.1%, and 84.4-114%, respectively. The method was applied to analyse 48 lentil samples from central Italy and pulses for determining the isoflavone content, which was found to range from 1.1 to 95.6 μg kg(-1)., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Biogenic amines (BAs) are considered to be important indicators of freshness and quality in food. In this work, an analytical method for analyzing ten underivatized BAs in meat by performance liquid chromatography-tandem mass spectrometry has been developed. Comparison between ion trap and triple quadrupole as mass analyzers indicated that the latter provides greater sensitivity and selectivity. The range of the correlation coefficients of the calibration curves of the analyzed compounds was 0.987-0.999, and the limits of detection and limits of quantification were in the range of 0.002-0.1 mg l(-1) and 0.008-0.5 mg l(-1), respectively. Once validated, the method was used to analyze the concentrations of BAs in 16 commercial meat samples, for evaluating the freshness of food through the study of BA indices, i.e. biogenic amine index (BAI) and the ratio spermidine/spermine (SPD/SPE). The results indicated that all the samples were fresh, with a BAI lower than 1.49 mg kg(-1) and a SPD/SPE ratio lower than 0.41 in each case. This methodology for testing the freshness of meat has potential for quality control applications along the entire production chain of meat products., (Copyright © 2014 John Wiley & Sons, Ltd.)

A new method for extracting isoflavones from espresso coffee (EC) was coupled with high-performance liquid chromatography- tandemmass spectrometry (MS/MS) for the first time to analyse five isoflavones, which included both a glycosilated form, genistin and the aglycons daidzein, genistein, formononetin and biochanin A. Isoflavones were extracted fromcoffee samples usingmethanol, stored in a freezer overnight to precipitate proteic or lipidic residues and purified on SPE C18 cartridges before highperformance liquid chromatography-MS/MS analysis. The recovery percentages obtained by spiking the matrix at concentrations of 10 and 100 μg l-1 with a standard mixture of isoflavones were in the range of 70 to 104%. The limits of detection and limits of quantification were in the range of 0.015-0.3 μg l-1 and 0.05-1 μg l-1, respectively. Once validated, the method was used to analyze the concentrations of isoflavones in six ECs and ten ground coffee samples. Only formononetin and biochanin A were found, and their respective concentrations ranged from 0.36 to 0.41 μg l-1 and from 0.58 to 3.26 μg l-1 in ECs and from 0.36 to 4.27 μgkg-1 and from 0.71 to 3.95 μgkg-1 in ground coffees. This method confirms the high specificity and selectivity of MS/MS systems for detecting bioactives in complex matrices such as coffee. [ABSTRACT FROM AUTHOR]

Two organic acids isomers, 3‐isopropylmalic acid (3‐IPMA) and 2‐isopropylmalic acid (2‐IPMA), were identified and quantified in wine samples by using an LC–MS/MS method without any chromatographic separation, but processing the MS/MS data with a recently developed deconvolution algorithm (LEDA: linear equations deconvolution analysis), thus decreasing the time necessary for the process. In particular, the LEDA tool processes the MS/MS signals and assigns the relative concentrations (abundances) of the isomers in the sample, at the mg L−1 level. The efficiency of MS/MS signal assignment was improved by introducing five linear equations to define the LEDA matrix. Then, as a novel approach, an overdetermined system of linear equations was applied for the deconvolution of isomers. The use of LEDA to identify and quantify the isomers in wine samples, together with the choice of a short LC column and a fast elution gradient, simplifies the process and shortens the time needed. Furthermore, it was evaluated the quantitative determination of the IPMA isomers by using the calibration curve provided by the precursor ion MRM transition data. The calculated values of accuracy (recovery between 82.6% and 99.8%) and precision (RSD between 0.4% and 4.0%) confirm the validity of this quantitative approach and the ability of LEDA to establish the correct percentage of the MS/MS signal for each isomer. Finally, to compare the conventional LC–MS/MS method and our proposed method of LC–MS/MS coupled with LEDA post‐processing elaboration, a series of real wine samples were analysed by both methods, and the results were compared. [ABSTRACT FROM AUTHOR]