Paraquat (PQ), has been used in many countries for controlling weed growth in agriculture because of its quick-acting and nonselective contact with green plant tissue.
A multiresidue analytical method was developed for grapes for the following 24 plant growth regulators: 1-naphthylacetamide, 2,3,5-triiodobenzoic acid, 2,4,5-T, 2-naphthoxyacetic acid, 3-indolylacetic acid, 4-(3-indolyl)-butyric acid, 4-chlorophenoxyacetic acid, 4-nitrophenol, 6-benzylaminopurine, N6-isopentenyladenine, butralin, chlormequat chloride, chlorphonim-Cl, cloprop, forchlorfenuron, gibberellic acid 3, gibberellic acid 4, gibberellic acid 7, inabenfide, mepiquat chloride, paclobutrazol, prohydrojasmon, thidiazuron and uniconizole-P. The compounds were extracted from grape samples using an extraction method modified from the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method. Liquid chromatography - tandem mass spectrometry was used for the detection and quantification of the compounds. Validation of the method was performed by using recovery studies at both intra-day and inter-day intervals, as well as by evaluation of the matrix effect, limit of quantification, trueness and precision. We used matrix-matched calibrations for the quantification of the compounds, which all resulted in determination coefficients (r) higher than 0.995. The limit of quantification ranged from 0.1 to 5 ng/mL. Recovery studies using three spiking concentrations at varying levels showed recoveries of 70.2-112.6% and 67.5-101.8% at intra-day and inter-day intervals, respectively. Relative standard deviations were below 20% for the recovery studies. The extraction method were further validated by performing recovery study and matrix effect test in six different grape varieties from Taiwan and the United States and all resulted in comparable results. Application of the established method to 50 grape samples, resulted in the detection of chlormequat chloride and forchlorfenuron residues in the tested grapes. The results of the method validation and real sample analysis shows the extraction method is therefore suitable for routine monitoring of residue in grapes.
Background: The quick, easy, cheap, effective, rugged, and safe method, generally applied to the determination of pesticide residues in food, has been recently modified and adopted for the analysis of pesticide residues worldwide, including Taiwan. Objective: The method still needs to be improved, particularly in efficiency and normalization, because the time costs 20–30 min for extraction and cleanup of multiple pesticides in every food. Methods: In this study, we present a highly efficient and simple sample preparation method that was developed for the determination of 380 pesticide residues in food, including mangoes, scallions, bok choy, apples, carrots, and pea seedlings. The homogenized 1 g samples mixed with 5 mL 1.0% acetic acid in acetonitrile were pushed through the FaPEx® (fast pesticide extraction) kits in a dropwise manner to obtain sample extracts. The total processing time was less than 15 min. The extracts were subject to chromatographic separation followed by GC–tandem MS (MS/MS) and LC–MS/MS analysis. Results: For more than 270 pesticide residues in these foods, the test gave acceptable mean recoveries, ranging between 70 and 120%, and relative SDs below 20%. The LOQ was at least 0.01 mg/kg for 380 pesticides. Conclusions: The developed method can greatly reduce the time needed for multiple pesticide residues analysis. Highlights: FaPEx is used for the extraction of pesticide residues that relies on single-use pre-filled sealed cartridges. FaPEx diminishes operation time, glassware demand, and laboratory space requirement. It also significantly decreases the amount of chemical solvents.
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