Journal
CHROMATOGRAPHIA
Volume 79, Issue 17-18, Pages 1113-1130Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s10337-016-3116-y
Keywords
High-throughput automation; Solid-phase extraction cleanup; Pesticide residue analysis; QuEChERS sample preparation; Fast GC-MS/MS; Analyte protectants; Environmental contaminants; Foods
Funding
- ARS [ARS-0430153, 911964] Funding Source: Federal RePORTER
Ask authors/readers for more resources
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 (LPGC-MS/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 A mu L for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO4/PSA (primary secondary amine)/C-18/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 aecurrency sign 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 + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.
Authors
I am an author on this paper
Click your name to claim this paper and add it to your profile.
Reviews
Recommended
No Data Available