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Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography-Tandem Mass Spectrometry.

ABSTRACT: A sensitive and reliable method was developed to determine methylene blue (MB) and its metabolite residues, including azure A (AZA), azure B (AZB), and azure C (AZC) in aquatic products by HPLC-MS/MS. The samples were extracted by acetonitrile and cleaned up by alumina-neutral (ALN) cartridges. The analytes were separated on a Sunfire C18 column (150 mm × 2.1 mm, 5 µm). The method was validated according to the European criteria of Commission Decision 2002/657/CE. Good linearity between 1-500 µg/L was obtained with correlation coefficients (R²) greater than 0.99. The limit of quantification (LOQ) was 1.0 µg/kg. The average recoveries at three levels of each compound (1, 5, and 10 µg/kg) were demonstrated to be in the range of 71.8-97.5%, with relative standard deviations (RSDs) from 1.05% to 8.63%. This method was suitable for the detection of methylene blue and its metabolite residues in aquatic products.

SUBMITTER: Zhang X

PROVIDER: S-EPMC8401997 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:Commercial viticulture necessitates regular pesticide applications to manage diseases and pests, raising significant concerns regarding pesticide residues among stakeholders. Due to health risks associated with these residues in Turkish vine leaves, the European Commission has increased the frequency of official control from 20% to 50%. Thus, the aim of this study was to determine multi-class pesticide residues in brined vine leaves from Turkey. A total of 766 samples of vine leaves were collected between May 2022 and June 2023. More than 500 residues were analyzed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, followed by liquid chromatography-tandem mass spectrometry. In-house validation data demonstrated that the analytical method exhibits fit-for-purpose performance in terms of linearity, accuracy, precision, and measurement uncertainty. Out of 766 samples analyzed, 180 samples (23.5%) contained one (131, 17.1%) or multiple (49, 6.4%) pesticides. Both the frequencies of occurrence and the rate of maximum residue level (MRL) exceedance increased in 2023 compared to 2022, with the MRL exceedance rate rising from 9.5% to 25.2%. Forty-three different residues were found in quantifiable concentrations and eight of them were non-approved. Among the residues, the non-systemic pyrethroid insecticides, lambda-cyhalothrin (8.0%) and cypermethrin (7.2%), were the two most frequently detected, with concentrations ranging from 0.010 to 0.248 mg kg-1 and from 0.011 to 0.533 mg kg-1, respectively. Turkey is a major exporter of vine leaves and these results provide crucial information regarding pesticide occurrence and quality assessment of vine leaves. The significant increase in both pesticide occurrence and MRL exceedance rates between 2022 and 2023 underscores the urgency for regulatory bodies to reassess current pesticide usage and monitoring practices. The findings emphasize the importance of implementing more stringent rules and improving enforcement methods in order to reduce the spread of unapproved pesticides and ensure adherence to global food safety standards.

Dataset Information

Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography-Tandem Mass Spectrometry.

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