Liquid Chromatography-Tandem Mass Spectrometry Detection of Human and Veterinary Drugs and Pesticides in Surface Water
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ABSTRACT:
SUBMITTER: Zhang X
PROVIDER: S-EPMC10593548 | biostudies-literature | 2023 Jan
REPOSITORIES: biostudies-literature
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Project description:IntroductionOcrelizumab is a monoclonal anti-CD20 antibody approved for the treatment of multiple sclerosis (MS). The clinical value of therapeutic drug monitoring (TDM) for this antibody in treatment of MS is unknown, and an adequately specific and precise quantitation method for ocrelizumab in patient serum could facilitate investigation. Liquid chromatography-tandem mass spectrometry (LC-MS/MS)-based quantitation methods have been shown to have higher analytic specificity and precision than enzyme-linked immunosorbent assays.ObjectivesTo establish and validate an LC-MS/MS-based quantitation method for ocrelizumab.MethodsWe present an LC-MS/MS-based quantitation method using immunocapture purification followed by trypsinization and analysis by a triple quadrupole mass analyzer obtaining results within the same day.ResultsWe found that the ocrelizumab peptide GLEWVGAIYPGNGDTSYNQK (Q1/Q3 Quantifier ion: 723.683+/590.77 y112+ Qualifier ion: 723.683+/672.30 y122+) can be used for quantitation and thereby developed a method for quantifying ocrelizumab in human serum with a quantitation range of 1.56 to 200 µg/mL. The method was validated in accordance with EMA requirements in terms of selectivity, carry-over, lower limit of quantitation, calibration curve, accuracy, precision and matrix effect. Ocrelizumab serum concentrations were measured in three MS patients treated with ocrelizumab, immediately before and after ocrelizumab infusion, with additional sampling after 2, 4, 8 and 12 weeks. Measured serum concentrations of ocrelizumab showed expected values for both Cmax and drug half-life over the sampled time period.ConclusionWe have established a reliable quantitation method for serum ocrelizumab that can be applied in clinical studies, facilitating the evaluation of ocrelizumab TDM in MS.
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Project description:Pesticide residues in aquatic products are of great concern due to the risk of environmental transmission and their extensive use in aquaculture. In our work, a quick screening approach was developed for the qualitative and semi-quantitative screening of 87 pesticide residues in aquatic products. The sample preparation was investigated, including extract solvent, extract methods, buffer salts, lipid removal, cleanup materials and filter membranes for aquatic products. Samples were extracted using a modified QuEChERS procedure, and two clean-up procedures were developed for UHPLC-Q/Orbitrap MS analysis based on the fat content of the aquatic products. The screening detection limits for all studied pesticides were distributed between 1 and 500 μg/kg in the three representative matrices. Seventy-one pesticides could be analyzed with a screening limit between 1 and 25 μg/kg in grass carp and crayfish, sixty-one pesticides could be screened for limits between 1 and 50 μg/kg in crab. The accuracy results showed that recoveries ranged from 50 to 120% for 60, 56 and 52 pesticides at medium-level for grass carp, crayfish and crab, respectively. At high spiking levels, 74, 65 and 59 pesticides were recovered within the range of 50-120% for the three matrices, respectively. The relative standard deviations of most compounds in different matrices were less than 20%. With this method, the local farmed aquatic products were tested for pesticide residues. In these samples, ethoxyquinoline, prometryn and phoxim were frequently detected. The majority of these confirmed compounds did not exceed 2.00 μg/kg. A grass carp with trichlorfon at 4.87 μg/kg and two carps with ethoxyquinoline at 200 µg/kg were detected, indicating the potential dietary risk.
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Project description:BackgroundKarrikins (KARs) are plant growth regulators that promote seed germination and the subsequent growth and development of seedlings of many plant species. In nature they are generated and released by combustion of plant material and promote the restoration of burned ecosystems. Smoke water can be artificially prepared as a saturated extract of all substances in smoke produced by burning plants, and it has various horticultural and agricultural applications.ResultsWe have developed, validated and applied the first fast, specific and sensitive method, based on ultra-high performance liquid chromatography-tandem mass spectrometry, for quantifying KARs in smoke water. To assist these efforts and further analyses, standards of the main KARs (which are not commercially available) were synthesized. Due to the complex matrix of smoke waters, two quantification approaches (standard dilution with a structural KAR analogue and standard addition) were compared. The standard addition method allowed absolute quantification of KARs in six of eight smoke water samples of diverse origins and ages.ConclusionsOur findings reveal differences in both total and relative levels of KARs in smoke water, and indicate that differences in its KAR composition may be linked to variations in its bioactivity.
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