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Sterols from Olive Oil on ZB-5MS

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:0.74 g olive oil in 10 ml 0.5 M KOH in ethanol. Shake and Reflux a 77 °C for 20 min. Cool down then add 10 ml 0.22 mg/ml betulin (istd) in chloroform and shake for 5 min. Let it settle and collect liquid phase in a 20 ml screw cap vial. Transfer and filter 3 ml aliquot to a BD 10 ml syringe screw to a Phenex 30 mm 0.45 um teflon filter, collect filtrate in 4 ml screw cap vial. Condition Strata C 18-E SPE (55 um, 70 A) on a manifold plugged to a vacuum pump, onto a 1/125 mm culture tube, with 5 ml methanol and 5 ml chloroform. Replaced tube with conditioning material with a new one and labeled accordingly, then transfer
onto miniscuos chloroform-sorbent 1 ml aliquot and elute sterols with 15 ml 5 % methanol in chloroform. Concentrate collected volume to 1 ml with nitrogen. Transfer 200 ul aliquot to 500 ul insert sample vial and dry completely with nitrogen,
reconstitute with 100 ul pyridine, and deirvatize with 100 ul BSTFA:TMCS; 99:1. Heat up at 70 °C for 20 min and inject.
Final Prep and Analysis: Intial Sample Unit: gram Inject: 0.5 µL on GC / Flame Ionization (FID) @ / (320 °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: 16515)

Part No:7HG-G010-11
Phase:5% Phenyl-Arylene 95% Dimethylpolysiloxane
Dimensions:30 meters x 0.25 mm x 0.25 µm
Oven Profile:225 °C to 330 °C @ 15 °C/min for 2 min.
Carrier Gas:Constant Flow Helium, 2.5 mL/min
Injection:Splitless :1 0.5 µL @ 320°C
Detection: Flame Ionization (FID) (320°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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