Determination of Sulfonamides in Milk Using Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry
This document details a method for extracting and analyzing trace levels of nine nitrogen-containing sulfa drugs in milk samples. The procedure utilizes Agilent SampliQ polymeric strong cation exchange (SCX) cartridges for solid-phase extraction (SPE) followed by separation and determination using an Agilent 6410 triple quadrupole LC/MS-MS system.
| Column Dimensions | 3.0 mm x 50 mm, 1.8 pm |
|---|---|
| Flow Rate | 0.42 mL/min |
| Column Temperature | 35 °C |
| Injection Volume | 1.7 pL |
| Gas Temperature | 350 °C |
| Gas Flow | 12 L/min |
| Capillary Voltage | 4000 V |
| Recovery Range | 73 to 99% |
| Limit of Detection Range | 0.2 to 2.0 ng/mL |
The method analyzes nine specific sulfa drugs: sulfamethoxazole, sulfadiazine, sulfathiazole, sulfamerazine, sulfamethizole, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, and sulfadimethoxine.
The analysis uses an Agilent 6410 triple quadrupole LC/MS-MS system coupled with an Agilent 1200 Series HPLC.
The run time for the separation is 8 minutes.
The limits of detection range from 0.2 to 2.0 ng/mL in milk, depending on the specific sulfa drug.