Application of Automated Mini–Solid-Phase Extraction Cleanup for the Analysis of Pesticides in Complex Spice Matrixes by GC-MS/MS. (29th January 2020)

• Record Type: Journal Article
• Authors: Goon, Arnab; Shinde, Raviraj; Ghosh, Bappa; Banerjee, Kaushik
• Is Part Of: Journal of AOAC International. Volume 103:Number 1(2020)
• Page Start: 40
• Page End: 45
• Publication Date: 2020-01-29
• Subjects: Agricultural chemistry -- Periodicals; Food -- Analysis -- Periodicals; 543
• DOI: 10.5740/jaoacint.19-0202
• Languages: English
• ISSNs: 1060-3271

Abstract

Abstract: Background: Pesticide residues are routinely tested in spices for trade compliance. This results in a huge sample load for food testing laboratories and demands automation in sample preparation. Although there exists a method for the analysis of pesticides in fruits using an automated sample cleanup by mini–solid-phase extraction (mini-SPE) technique, no study is available to date on spices. Objective: This study aims to develop an automated sample cleanup method using mini-SPE technique in a range of spices, including chili powder, turmeric, black pepper, cumin, coriander, and cardamom. Methods: This automated sample preparation workflow involved an X-Y-Z instrument autosampler, and a set of mini-SPE cartridges comprising cleanup sorbents. Spice samples were extracted by acetonitrile, and the extract was put into an autosampler vial for automated mini-SPE cleanup before analysis by GC tandem MS. For an efficient cleanup, three different sorbent compositions were compared along with various automated workflows. Results: For the relatively simple matrixes (e.g., coriander, cumin, and cardamom), the LOQ for the target pesticides was 10 ng/g with acceptable recovery, and precision. The method provided an LOQ of 10 ng/g for around 77% of the compounds in the relatively complex matrixes (e.g., turmeric, chili powder, and black pepper). The remainder of the compounds had satisfactory recoveries at 20 ng/g and higher levels. Conclusions: Given its time effectiveness and efficient analytical performance, this method can be adopted in commercial food testing laboratories for time-bound analysis of a large volume of samples. Highlights: The study describes effectiveness of the automated mini-SPE cleanup in multiresidue analysis of pesticides in a range of spice matrixes. The method facilitates high-throughput residue analysis in compliance with the regulatory requirements of sensitivity and method performance.