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Melamine and Cyanuric Acid Extracted from Baby Formula on ZB-XLB-HT by MSD

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 100 uL 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 50 uL 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.)
Final Prep and Analysis: Inject: 0.1 µL on GC / Mass Selective (MSD) @ amu / (325 °C)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
1 Cyanuric acid 13C3
2 Cyanuric acid
3 Melamine 13C3 15N3
4 Melamine

Application Detail (App ID: 18265)

Part No:7EG-G024-11
Phase:Proprietary XLB Phase
Dimensions:15 meters x 0.25 mm x 0.25 µm
Oven Profile:100 °C for 0.5 min to 320 °C @ 25 °C/min
Carrier Gas:Constant Flow Helium, 1.4 mL/min
Injection:On-Column :1 0.1 µL @ 103°C
Detection: Mass Selective (MSD) (325°C)
Note:Analytes are 200ng/100uL in BSTFA/Pyridine (1:1)
SIM Ions: Cyanuric Acid (IS) - 348*, 333, 101; Cyanuric Acid - 345*, 330, 100; Melamine (IS) - 173*, 333, 348; Melamine - 171*, 327, 342

Analyte Details

Analyte Detail not available

1
Cyanuric acid 13C3
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2
Cyanuric acid
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3
Melamine 13C3 15N3
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4
Melamine
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