UHPLC-HRMS (Orbitrap) polyphenolic profiling was applied to the characterization, classification, and authentication of cranberry-based natural and pharmaceutical products. Fifty three polyphenolic standards were characterized to build a user-accurate mass database which was then proposed to obtain UHPLC-HRMS polyphenolic profiles by means of ExactFinder software. Principal component analysis results showed a good sample discrimination according to the fruit employed. Regarding cranberry-based pharmaceuticals, discrimination according to the presentation format (syrup, sachets, capsules, etc.) was also observed due to the enhancement of some polyphenols by purification and preconcentration procedures. Procyanidin A2 and homogentisic, sinapic, veratric, cryptochlorogenic, and caffeic acids showed to be important polyphenols to achieve cranberry-based products discrimination against the other studied fruits. Partial least-squares regression allowed the determination of adulterant percentages in cranberry-fruit samples. Very satisfactory results with adulteration quantification errors lower than 6.0% were obtained even at low adulteration levels.
An analytical method has been developed for the simultaneous determination of seven benzotriazole, five benzothiazole and four benzenesulfonamide derivatives in surface water samples. The procedure is based on solid‐phase extraction with Oasis HLB, followed by high‐performance liquid chromatography coupled to high‐resolution mass spectrometry. Apparent recoveries ranged from 40 to 101%, except for compounds the matrix effect of which was above ‐60%. The repeatability (n = 5) of the method was below 20% for all compounds except 4‐hydroxybenzotriazole in river water. The method limits of detection for most compounds ranged from 1 to 12 ng/L for both river water and seawater. The method was then used for the determination of the studied compounds in several river water and seawater samples from harbour and coastal areas. 1‐H‐Benzotriazole (up to 78 ng/L in river water and above the upper limit of the calibration curve in seawater) and 4‐methyl‐1‐H‐benzotriazole (up to 44 ng/L in river water and 338 ng/L in seawater) were the most abundant compounds quantified in the samples, even though 5‐methyl‐1‐H‐benzotriazole and 2‐hydroxybenzothiazole were also found in most samples. Some compounds were frequently found in certain types of samples, such as 2‐aminobenzothiazole in river water. Benzenesulfonamide derivatives could not be quantified in any sample.
Organophosphate triesters are compounds widely used in industries and are ubiquitous in the environment, where they can be transformed into organophosphate diesters. Some organophosphate diesters are also used by industry. Several studies suggest organophosphate diesters can have toxic effects for reproduction, and hazardous and mutagenic properties. Due to the impact these compounds can have on marine biota and human beings through the consumption of fish and shellfish, it is necessary to study their presence in widely consumed seafood species. We therefore developed an analytical method for determining six of the most common organophosphate diesters in seafood. The procedure is based on the Quick, Easy, Cheap, Effective, Rugged and Safe extraction method and a solid phase extraction clean-up, followed by liquid chromatography coupled to high-resolution mass spectrometry. The method was optimised and validated for seafood with different lipid content, providing satisfactory relative recoveries (from 89 to 138%) and limits of detection (1.0–50 ng g−1 dry weight), as well as repeatability values (RSD% (n = 5, 100 ng g−1 (dry weight)) lower than 15%. Eight seafood species were analysed using this method and two organophosphate diesters were detected and quantified in all the samples, demonstrating the suitability of the method.
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