Simultaneous Extraction of Melamine and Cyanuric acid from Strata Melamine on Luna HILIC

Sample Preparation Details

Part No:8B-S049-FBJ
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:Protein Precipitation:
Weigh 0.2 g (200 mg) of Baby formula (Enfamil) in a 15 mL plastic centrifuge tube, add 1 mL Lukewarm water to make a homogeneous mix, vortex and add 100uL of 0.2N HCl followed by addition of 50 uL of 4.0 ug/mL of individual stock solution of melamine and cyanuric acid and 50uL of each internal standard (at 15.0 ug/mL).
Vortex 3-5 secs.
Add 3 mL of ACN, vortex and centrifuge at 6000Xg for 10 mins and then collect the supernatant to carry out SPE in the subsequent step. (Spiked conc. of analyte = 200 ng, IS spiked conc.= 750 ng; pH of sample is 5.5; melamine amino-15N3, and Cyanuric-13C3 used as I.S.)
Dry:2 mins at 10" of Hg
Final Prep and Analysis: Inject: 15 µL on HPLC / Mass Spectrometer (MS) @ (ambient)


Name Spiked
Log P pKa % Rec %RSC (n=0)
1 Cyanuric acid 200  68 4.1
2 Melamine 200  67 3.05

Application Detail (App ID: 18287)

Part No:00D-4449-B0
Dimensions:100 x 2 mm ID
Elution Type:Isocratic
Elution A:90/10 ACN/100 mM Ammonium Formate, pH 3.2
Gradient Profile:
Step No. Time (min) Pct A
1 3.5 100

Flow Rate:0.4 mL/min
Col. Temp: ambient
Detection: Mass Spectrometer (MS) @ (22°C)
Detector Info: * MS in -ve ionization till 1.7 mins then to +ve till 3.5 mins
Note:SecurityGuard™ Guard Cartridge System extends column lifetime.
- SecurityGuard Cartridges, HILIC 4 x 2.0mm, 10/Pk Part No.: AJ0-8328
- Holder Part No.: KJ0-4282

Analyte Details

Analyte Detail not available

Cyanuric acid