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Articles

Determination of quinclorac and quinclorac methyl ester in honey by online SPE-UPLC-MS/MS

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Pages 60-73 | Received 09 Aug 2023, Accepted 23 Nov 2023, Published online: 04 Dec 2023
 

Abstract

A method employing online solid phase extraction (SPE) coupled to UPLC-MS/MS was developed for the determination of residues of the acid herbicide quinclorac plus its transformation product, quinclorac methyl ester, in honey. The analytical method involved dissolving the honey in a mixture of methanol:water followed by direct injection into a two-dimensional UPLC system which is used to perform an automated SPE cleanup on a reusable phenyl cartridge prior to the target analytes being transferred onto an analytical UPLC column for subsequent chromatographic separation followed by MS/MS detection. The limits of quantitation for quinclorac and quinclorac methyl ester in honey were both set at 0.5 µg kg−1 and the method detection limit was estimated to be 0.012 µg kg−1 for each compound. The working analytical range (0.5–100 µg kg−1) was validated by analysing a series of spiked replicate honey samples. The method was applied to the analysis of various honeys obtained from numerous different commercial sources. Quinclorac was detected in 9 out of 30 samples at concentrations ranging from 0.6 to 31.5 µg kg−1. Quinclorac methyl ester, which is estimated to be significantly more toxic than the parent herbicide itself, was not detected in any honey sample.

Disclosure statement

No potential conflict of interest was reported by the author(s).

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