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  • A QuEChERS-Based Sample Preparation Method for the Analysis of 5-Nitroimidazoles in Bovine Milk by HPLC-DAD.

A QuEChERS-Based Sample Preparation Method for the Analysis of 5-Nitroimidazoles in Bovine Milk by HPLC-DAD.

Journal of AOAC International (2017-07-15)
Tomasz Tuzimski, Tomasz Rejczak
ABSTRACT

In this study, a simple, cost-effective, and sensitive HPLC diode-array detection method was developed for the simultaneous determination of six different 5-nitroimidazoles [metronidazole, 2-hydroxymethyl-1-methyl-5-nitro-1H-imidazole, dimetridazole (DMZ), ronidazole, ornidazole, and ipronidazole] in bovine milk samples. A QuEChERS-based sample preparation procedure was optimized by evaluating different cleanup sorbents, including zirconium-based sorbents (Z-Sep and Z-Sep+), C18, and primary-secondary amine (PSA), as well as EMR-Lipid cleanup solution. Acceptable analytical performance for all analytes was observed with recoveries in the range of 45-93% and RSDs of less than 15%. Negligible matrix interference was observed for most of the analytes due to application of PSA sorbent in a dispersive solid-phase extraction cleanup step. Method LOQs (mLOQs) for five of the six investigated analytes were set at a satisfactory low food product value of 2.5 ng/mL. For DMZ only, the mLOQ was set at 10 ng/mL. The procedure was evaluated through the analysis of 10 different natural samples.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, Z-Sep+ Bulk, pkg of 20 g
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 12 mL, pack of 50 ea
Supelco
Supel QuE, Z-Sep+ Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, centrifuge tube volume 2 mL, pack of 100 ea
Supelco
Supel QuE, Z-Sep/C18 Tube, centrifuge tube volume 2 mL, pack of 100
Supelco
HMMNI, VETRANAL®, analytical standard
Supelco
Supel QuE, Z-Sep+ with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep+ Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep with MgSO4 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep/C18 Tube, pk of 50, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, Z-Sep Bulk