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Sulfonamide by LCMS
An MS Friendly Method

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Note: Sulfonamides are used for the treatment of infections and promotion of growth of livestock and fish. The residue of these veterinary drugs in food is of serious concern, due to the risk to human health (resistance to drugs and allergic or toxic reactions).


Method Conditions



Column Cogent Bidentate™, 4µm, 100A
Catalog No. 40018-75P
Dimensions 4.6 x 75 mm
Mobile Phase Reverse Phase Gradient:
Solvent A: 100% DI water + 0.1% formic acid
Solvent B: 100% acetonitrile

Time %A %B
0.00 70 30
0.00-0.20 70 30
0.20-5.00 0 100
5.00-10.00 0 100
10.00-10.01 70 30
10.01-15.00 70 30
Flow rate 1.0 mL/minute
Injection Volume  10 µL
Peak 1mg of the compound dissolved in 1 mL of substituted sulfonamide (m/z 468) concentration for UV
Analysis 0.5 mg/mL and for LC/MS: 0.1 mg/mL
Detection A: UV 259 nm
B: LC/MS: Atmospheric Pressure
  Chemical Ionization in positive mode: APCI+, Single Ion Monitoring


Discussion


The current sulfonamide detection methods are based on UV absorption, but there is a need for methods detecting residues below the maximum residue limits (MRL). LC/MS is a method of choice. A simple and quick RP gradient was used to transfer the HPLC/UV method to LC/MS for analysis of basic sulfonamides. APCI ionization mode was more advantageous than ESI.






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