The automated mini-SPE cleanup coupled with GCMSMS analysis not only achieved high quality results for diverse type of analytes and foods, the approach also enabled reliable, high-throughput operations without much labor or instrument maintenance.

This paper was written by Steven J. Lehotay, Lijun Han and Yelena Sapozhnikova.

Received: 8 April 2016 / Accepted: 24 May 2016 / Published online: 13 June 2016

Abstract

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography—tandem mass spectrometry (LPGCMS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO4/PSA (primary secondary amine)/C18/CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g−1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70–120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices (n = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGCMS/MS method yielded accurate results in rugged, highthroughput operations with minimal labor and data review.