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Extraction of Sulfonamides from Honey by LC/MS/MS Using strata X-C and Gemini 5u, C18, 150x3.0

Sample Preparation Details

Part No:8B-S029-UBJ
Solid Phase Extraction (SPE) procedure:Note: The solvent volumes shown below are for a 60 mg bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass.
Load:Sample load: 5 ml analyte spiked diluted Honey sample processed in the following manner:
1gm honey +1 mL of 2.0M HCl, leave it with 30 mins of sonication; add 0.3M citric acid solution to make upto the volume of 5mL
Dry:2 mins at 10" of Hg pressure
Final Prep and Analysis: Addition of IS followed by evaporation before reconstitution:
Add IS (Sulfaquinoxaline) and evaporate the sample under slow stream of nitrogen @ 40 deg C and reconstitute with 100 uL of mobile phase

Inject: 10 µL on HPLC / Mass Spectrometer (MS) @ amu (ambient)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
1 Sulfanilamide 100  -0.62 34
2 Sulfathiazole 100  0.09 81
3 Sulfamerazine 100  0.54 78
4 Sulfamethoxazole 100  1.58 94
5 Sulfaquinoxaline 100  1.68

Application Detail (App ID: 18458)

Part No:00F-4435-Y0
Dimensions:150 x 3 mm ID
Elution Type:Gradient
Elution A:0.1% Formic acid/water
Elution B:0.1% formic acid/ACN
Gradient Profile:
Step No. Time (min) Pct A Pct B
1 0 90 10
2 8 30 70

Flow Rate:0.6 mL/min
Col. Temp: ambient
Detection: Mass Spectrometer (MS) @ amu (22°C)
Note:HPLC system: HP 1100 MS detector: API 3000, LC/MS/MS,Turbo spray: ESI, positive ion mode; MRM; heater gas flow 7000 cc/min; heater temp: 425° C

Analyte Details

Analyte Detail not available

1
Sulfanilamide
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2
Sulfathiazole
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3
Sulfamerazine
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4
Sulfamethoxazole
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5
Sulfaquinoxaline
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