Application of Automated Mini–Solid-Phase Extraction Cleanup for the Analysis of Pesticides in Complex Spice Matrixes by GC-MS/MS

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.

Automation in Pesticide Residue Analysis in Foods: A Step toward Smarter Laboratories and Green Chemistry

“…Using micro - SPE (Figure ), the method efficiency and laboratory throughput can be significantly increased. This automated technology cleans raw extracts using micro-SPE cartridges that are compatible with a variety of commodities, including spices , and fatty matrices . Using an x,y,z-robotic autosampler, loading the raw extract onto a cartridge and its subsequent elution have become simple and require less human involvement.…”

Assessing the performance of various sorbents in micro-solid phase extraction cartridges for pesticide residue analysis in feed

“…To reduce labor and improve precision, laboratory automation has been implemented through the utilization of robotic sample preparation tools in sample cleanup. 18 The micro-solid-phase-extraction (mSPE) clean-up method is a clean-up process, where the sample extract is delivered via a syringe at the desired volume and ow rate. The unwanted matrix components are retained on the cartridge, while the compounds of interest are eluted from the column.…”

“…In the following years, the use of mSPE clean-up was demonstrated to be effective for the analysis of pesticide residues in different commodities such as cereals, sh, lamb, hemp, tea, and spice. 6,18,[22][23][24][25][26][27][28][29] A current drawback of mSPE cartridges is a lack of different sorbent packings.…”