GC Analysis of Polynuclear Aromatic Hydrocarbons (PAHs) in Butter on SLB®-35ms after SPE using Supelclean™ EZ-POP NP
材料
used together
CONDITIONS
sample preparation
SPE (Solid Phase Extraction)
sample/matrix
butter
SPE tube/cartridge
Supelclean EZ-POP NP, 2.5 g/12 mL (54341-U)
extraction process
0.5 gm melted butter, diluted to 1 mL in cyclohexane
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
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
column
SLB-35ms, 30 m x 0.25 mm I.D., 0.25 μm (29804-U)
oven
60°C (1 min), 20 °C/min to 340°C (10 min)
inj. temp.
300 °C
detector
MSD-SIM (MS source temp.: 250°, MS quads temp.: 200°C)
MSD interface
330 °C
scan range
SIM
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
说明
分析说明
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.
其他说明
Sample pretreatment: 0.5 gm melted butter, diluted to 1 mL in cyclohexane
法律信息
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany
Supelclean is a trademark of Sigma-Aldrich Co. LLC