Extraction of Sulfonamides from Honey by LC/MS/MS Using strata X-C and Gemini 5u, C18, 150x3.0
LC Conditions
Column
Gemini 5 µm C18 110 Å, LC Column 150 x 3 mm, Ea
Brand
Gemini
Part No
00F-4435-Y0
Phase Name
C18
Elution Type
Gradient
Mobile Phase
A: 0.1% Formic acid/water
B: 0.1% formic acid/ACN
Gradient Profile
Step No.
Time(min)
%A
%B
1
0
90
10
2
8
30
70
Flow Rate
0.60 mL/min
Temperature
22°C
Detection
Mass Spectrometer (MS) @ (22°C)
Detection Info
Sample Notes
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
Sample Preparation Details
Description
Strata-X-C 33 µm Polymeric Strong Cation, 60 mg / 3 mL, Tubes, 50/Pk
Part No
8B-S029-UBJ
Pretreatment Note
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
Condition 1
2 mL Methanol at 1 mL/min
Condition 2
2 mL Water at 1 mL/min
Load
Load 1.00 mL Sample diluted in 1mL of 2M HCl and 3mL 0.3M Citric acid
Wash 1
4 mL Water (2 aliquots of 2 mL) at 1 mL/min
Wash 2
4 mL MeOH/ACN (50/50) (2 aliquots of 2 mL) at 1 mL/min
Dry
2 mins at 10 of Hg pressure
Elution 1
2 mL 2% ammonium hydroxide/MeOH at 1 mL/min
Evaporation
Evaporate to dryness
Reconstitute
0 µL Mobile Phase
Order Items Used in This Application
- 1. Sulfanilamide
- 2. Sulfathiazole
- 3. Sulfamerazine
- 4. Sulfamethoxazole
- 5. Sulfaquinoxaline
-OEChem-06211003152D<br><br> 19 19 0 0 0 0 0 0 0999 V2000<br> 3.0000 1.5000 0.0000 S 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.0000 1.5000 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.0000 1.5000 0.0000 O 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.0000 2.5000 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.0000 -2.5000 0.0000 N 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.0000 0.5000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.8660 0.0000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.1340 0.0000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.0000 -1.5000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.8660 -1.0000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.1340 -1.0000 0.0000 C 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.4030 0.3100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 1.5970 0.3100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 4.4030 -1.3100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 1.5970 -1.3100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.5369 2.8100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.4631 2.8100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 2.4631 -2.8100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 3.5369 -2.8100 0.0000 H 0 0 0 0 0 0 0 0 0 0 0 0<br> 1 2 2 0 0 0 0<br> 1 3 2 0 0 0 0<br> 1 4 1 0 0 0 0<br> 1 6 1 0 0 0 0<br> 4 16 1 0 0 0 0<br> 4 17 1 0 0 0 0<br> 5 9 1 0 0 0 0<br> 5 18 1 0 0 0 0<br> 5 19 1 0 0 0 0<br> 6 7 2 0 0 0 0<br> 6 8 1 0 0 0 0<br> 7 10 1 0 0 0 0<br> 7 12 1 0 0 0 0<br> 8 11 2 0 0 0 0<br> 8 13 1 0 0 0 0<br> 9 10 2 0 0 0 0<br> 9 11 1 0 0 0 0<br> 10 14 1 0 0 0 0<br> 11 15 1 0 0 0 0<br>M END
Compound Name
Sulfanilamide
CID
5333
Molecular Formula
C6H8N2O2S
Molecular Weight
172
No. Hydrogen Bond Acceptors
4
No. Hydrogen Bond Donors
2
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