GC Analysis of Polynuclear Aromatic Hydrocarbons (PAHs) in Butter on SLB®-35ms after SPE using Supelclean™ EZ-POP NP

GC Analysis of Polynuclear Aromatic Hydrocarbons (PAHs) in Butter on SLB®-35ms after SPE using Supelclean™ EZ-POP NP

Conditions

sample preparation Supelclean LC-Si, 500 mg/3 mL, condition: 3 mL acetone, dry 10 min; then 6 mL hexane, load: concentrated hexane extract, elute: 10 mL hexane, concentrate extract to 1 mL
sample preparation SPE (Solid Phase Extraction)
sample/matrix butter
extraction process 0.5 gm melted butter, diluted to 1 mL in cyclohexane
SPE tube/cartridge Supelclean EZ-POP NP, 2.5 g/12 mL (54341-U)
condition 10 mL acetone, dry 10 min at -10 to -15" Hg
sample addition 0.5 mL butter in cyclohexane
elution 2 x 10 mL acetonitrile
eluate post-treatment add 5 mL water to eluant, and backextract with 2 x 10 mL aliquots of hexane. concentrate hexane extract to 1 mL
column SLB-35ms, 30 m x 0.25 mm I.D., 0.25 µm (29804-U)
oven 60C (1 min), 20 C/min to 340C (10 min)
carrier gas helium, 1 ml/min constant flow
injection 0.5 µl pulsed splitless (60 psi until 0.75 min; splitter open at 0.75 min)
liner 2 mm I.D. FocusLiner with taper
inj. temp. 300 C
detector MSD-SIM (MS source temp.: 250, MS quads temp.: 200C)
MSD interface 330 C
scan range SIM

Description

Analysis Note PAHs are ubiquitous in the environment, resulting from both natural and manmade sources of combustion. Farm animals such as cows can become exposed to them through both consumption of contaminated feed and water, and inhalation of contaminated atmosphere. Consequently, these compounds can be present in dairy products produced from cow’s milk such as cheese and butter.
In this application, EZ-POP NP SPE was used as part of an extraction and cleanup procedure for the analysis of PAHs in butter by GC/MS-SIM. After EZ-POP NP extraction, a secondary cleanup was done using silica gel. This produced an extract with low GC/MS background.
Categories Analytical Chromatography, SPE Applications, GC Applications, Hydrocarbons, PAHs
Featured Industry Food and Beverages
Legal Information Supelclean is a trademark of Sigma-Aldrich Co. LLC, SLB is a registered trademark of Sigma-Aldrich Co. LLC
Other Notes Sample pretreatment: 0.5 gm melted butter, diluted to 1 mL in cyclohexane
suitability application for GC, application for SPE

Materials

     
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