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Fluoroquinolones by LCMS using Kinetex C8 2.6µm, 50 x 2.1 mm

Sample Preparation Details

Part No:8B-S100-FCH
Solid Phase Extraction (SPE) procedure:Note: The solvent volumes shown below are for a 200 mg bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass.
Load:Dissolve 125mg of propolis in 5mL of MTBE.
Using Phosphate buffer with 2% TCA, extract analytes from propolis by
2X liquid:liquid extraction.
Aqueous fraction is then ready for loading onto SPE cartridge.
Dry:5min @ >10 in Hg
Final Prep and Analysis: Inject: 20 µL on HPLC / Mass Spectrometer (MS) @ amu (550 °C)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
1 Ofloxacin 25 
2 Norfloxacin 25 
3 Norfloxacin-d5 25 
4 Ciprofloxacin 25 
5 Ciprofloxacin-d8 25 
6 Enrofloxacin 25 
7 Difloxacin 25 
8 Sparfloxacin 25 

Application Detail (App ID: 19655)

Part No:00B-4497-AN
Dimensions:50 x 2.1 mm ID
Elution Type:Gradient
Elution A:0.1% Formic acid
Elution B:Methanol
Gradient Profile:
Step No. Time (min) Pct A Pct B
1 0 85 15
2 5 10 90
3 6 10 90
4 6 10 90

Flow Rate:0.4 mL/min
Col. Temp: 40 °C
Detection: Mass Spectrometer (MS) @ amu (550°C)
Detector Info: AB Sciex API 4000™
Note:Source temp: 550ºC
Polarity: Postive
Dwell: 25 msec

Analyte Details

Analyte Detail not available

1
Ofloxacin
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2
Norfloxacin
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3
Norfloxacin-d5
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4
Ciprofloxacin
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5
Ciprofloxacin-d8
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6
Enrofloxacin
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7
Difloxacin
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8
Sparfloxacin
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