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Sterols from Margarine by FID on ZB-5HT

Sample Preparation Details

Part No:8B-S001-JCH
Solid Phase Extraction (SPE) procedure:Note: The solvent volumes shown below are for a 1 g bed mass. The solvent volumes will need to be adjusted for a smaller or larger bed mass.
Load:Saponify sample in 10 mL 0.5 M KOH in ethanol at 77 °C for 20 min.
When cool, add 10 mL of 0.22 mg/ml betulin (istd) in chloroform and shake.
Adjust 3 mL aliquot of sample to pH 2.5 with 5 M HCl.
Syringe filter aliquot through Phenex 30 mm 0.45 um teflon filter.
Purify via Strata C18-E (55 um, 70 A).
[Condition SPE with 5 mL methanol then 5 mL chloroform.
Load 1 mL of filtrate sample.
Elute with 15 mL 5% methanol in chloroform.]
Blow down eluate to 1 mL.
Transfer 200 µL to 500 µL insert and dry under nitrogen.
Reconstitute with 100µL pyridine and 100 ul BSTFA:TMCS 99:1 and derivatize at 70C for 20 min.
Final Prep and Analysis: Initial Sample Weight / Unit: 0.70 grams Inject: 0.5 µL on GC / Flame Ionization (FID) @ / (350 °C)

Analytes:

Name Spiked
Conc.
Log P pKa % Rec %RSC (n=0)
1 Campesterol
2 Stigmasterol
3 b-Sitosterol
4 Betulin

Application Detail (App ID: 16750)

Part No:7HG-G015-02
Phase:5% Phenyl 95% Dimethylpolysiloxane
Dimensions:30 meters x 0.25 mm x 0.1 µm
Oven Profile:220 °C to 350 °C @ 15 °C/min.
Carrier Gas:Constant Flow Helium, 2 mL/min
Injection:Splitless :1 0.5 µL @ 350°C
Detection: Flame Ionization (FID) (350°C)
Note:Sample Prep: Saponification, Solid Phase Extraction (SPE), and Derivatization.

Analyte Details

Analyte Detail not available

1
Campesterol
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2
Stigmasterol
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3
b-Sitosterol
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4
Betulin
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