Abstract
Food analysis is a tremendously broad field that is constantly evolving. New methods have emerged to increase productivity, such as modern miniaturized and robotic analytical techniques. In this paper, a micro-solid-phase extraction system (µ-SPE) for clean-up was combined with a robotic autosampler to yield ready-to-analyze extracts. The system was evaluated for its applicability in routine laboratories. The new, automated, high-throughput µ-SPE clean-up method was applied to acetonitrile extracts and was developed for the analysis of pesticide residues in cereals by gas chromatography-Orbitrap mass spectrometry (GC-Orbitrap-MS). The µ-SPE clean-up efficiency was demonstrated in the removal of matrix-interfering components and in the recovery of pesticides. The sorbent bed mixture consisted of magnesium sulfate, primary-secondary amine, C18, and CarbonX, and effectively retained matrix components without loss of target analytes. Analysis of five types of cereals (barley, oat, rice, rye, and wheat) by GC-Orbitrap-MS showed that the method removed more than 70% of matrix components. The clean-up method was validated for 170 pesticides in rye, 159 pesticides in wheat, 142 pesticides in barley, 130 pesticides in oat, and 127 pesticides in rice. Spike recovery values were 70–120% for all pesticides and the repeatability, calculated as the relative standard deviation, was less than 20%. The limits of quantitation achieved were 0.005 mg kg−1 for almost all analytes, ensuring compliance with the maximum residue limits.
Highlights
Pesticide residues, among the large variety of contaminants, are continuously monitored and controlled to ensure legislative compliance
Pesticide residue analysis is crucial in estimating maximum residue limits, reviewing toxicological data, and ensuring food safety
The objective of this study was to evaluate the performance of the automated μ-SPE technique in the analysis of 172 pesticide residues in cereals, and to determine if the technique could be used in national and official routine analysis laboratories
Summary
Among the large variety of contaminants, are continuously monitored and controlled to ensure legislative compliance. Pesticide residue analysis is crucial in estimating maximum residue limits, reviewing toxicological data, and ensuring food safety. Similar to other food analysis applications, the sample preparation step is often the key parameter in method development, in the isolation and detection of contaminants. Besides the accuracy and validity of the method, the time required to complete the analytical process and the cost of the consumables (e.g., solvents and sorbents) used in the analysis are considered. It is estimated that 60–80% of the work activity and operational costs in analytical laboratories are spent preparing samples for analysis. It is estimated that this step is responsible of 50% of the error in the final reported data [20].
Sign-in/Register to view highlights & summary Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
