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  • Capillary electrophoresis-mass spectrometry as a new approach to analyze neonicotinoid insecticides.

Capillary electrophoresis-mass spectrometry as a new approach to analyze neonicotinoid insecticides.

Journal of chromatography. A (2014-08-03)
Laura Sánchez-Hernández, Deamelys Hernández-Domínguez, José Bernal, Christian Neusüß, María T Martín, José L Bernal
ABSTRACT

This paper represents the first report of a capillary electrophoresis (CE) method compatible with mass spectrometry (MS) detection for simultaneously analyzing seven neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid and thiamethoxam). Different variables affecting CE separation (buffer concentration, pH, applied voltage and injection time) and MS detection (electrospray parameters) were studied. Low limits of detection (LOD) and quantification (LOQ) were achieved for all analytes, ranging from 1.0 to 2.3μg/L, and from 3.5 to 7.2μg/L, respectively. In addition, the proposed method showed itself to be linear in the range from LOQ to 1000μg/L and to be precise, as the relative standard deviations of the migration times were lower than 4% in all cases. Finally, the proposed CE-MS method was applied to assess the efficacy of a beeswax cleaning treatment with oxalic acid to remove residues of three of the most commonly used neonicotinoids (clothianidin, imidacloprid and thiamethoxam), use of which has recently been restricted by the European Union.

MATERIALS
Product Number
Brand
Product Description

Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
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Methanol, suitable for NMR (reference standard)
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Acetic acid, ≥99.5%, FCC, FG
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Acetic acid-12C2, 99.9 atom % 12C
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Acetic acid, natural, ≥99.5%, FG
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Ammonium acetate, BioUltra, ≥99.0%
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Sodium hydroxide, BioUltra, suitable for luminescence, ≥98.0% (T), pellets
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Sodium hydroxide solution, 49-51% in water, eluent for IC
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Sodium hydroxide solution, BioUltra, Molecular Biology, 10 M in H2O
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Acetic acid, suitable for luminescence, BioUltra, ≥99.5% (GC)
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Methanol, anhydrous, 99.8%
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Ammonium acetate solution, Molecular Biology, 7.5 M
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Ammonium acetate, BioXtra, ≥98%
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Ammonium acetate, Molecular Biology, ≥98%
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Ammonium acetate, reagent grade, ≥98%
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Methanol, purification grade, 99.8%
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Ammonia-14N, 99.99 atom % 14N
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Ammonium acetate, LiChropur, eluent additive for LC-MS
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Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, 99.8-100.5%
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Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
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Methanol, Laboratory Reagent, ≥99.6%
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Ammonium acetate solution, BioUltra, ~5 M in H2O
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Supelco
Methanol, analytical standard
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Thiacloprid, PESTANAL®, analytical standard
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Acetic acid, analytical standard
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Ammonium acetate, 99.999% trace metals basis
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Isopropyl alcohol, ≥99.7%, FCC, FG
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Sodium hydroxide, reagent grade, 97%, powder