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Key Documents

G003760

Fractionation of cis/trans FAMEs in popcorn oil

application for SPE, suitable for GC

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About This Item

technique(s)

gas chromatography (GC): suitable
solid phase extraction (SPE): suitable

test parameters

sample preparation: SPE (Solid Phase Extraction)
sample/matrix: 1 g of popcorn oil FAME′s in Hexane
SPE tube/cartridge: Discovery Ag-Ion, 750 mg/6 mL (54225-U)
condition: 4 mL acetone and 4 mL hexane
sample addition: 1 mL of the hexane FAME extract
elution: 6 mL hexane:acetone (96:4, v/v) followed by 4 mL hexane:acetone (90:10, v/v)
column: SP-2560, 75 m x 0.18mm I.D., 0.14 μm (23348-U)
oven: 180 °C isothermal
inj. temp.: 220 °C
detector: FID, 220 °C
carrier gas: hydrogen, 40 cm/sec. at 180 °C
injection: (0.5 μL, 100:1 split)
liner: 0.5 μL, 100:1 split

suitability

application for SPE

application(s)

agriculture
food and beverages

Preparation Note

Sample pretreatment: A 1 g sample of popcorn oil was scraped from the inside of a popped microwave oven popcorn bag and mixed with 8 mL deionized water (DI) and 4 mL petroleum ether, centrifuged to remove particulates. The ether layer (upper layer) was collected. This petroleum ether extraction step was repeated four times. The upper ether layers were combined, evaporated, and reconstituted in 16 mL toluene. A 1 mL aliquot was transferred to conical reaction vial and 2 mL 7% boron triflluoride in methanol were added. The reaction was incubated at 80 °C for 15 minutes using a heating block, then cooled to room temperature. 1 mL DI water was added and FAMEs were extracted twice using 1 mL hexane each time. The upper hexane layers were combined into a fresh vial, evaporated, and reconstituted in 5 mL hexane and 50 mg anhydrous sodium sulfate.

Analysis Note

Discovery Ag-Ion operates by argentation chromatography which is a powerful analytical and sample prep technique for the separation or fractionation of cis and trans geometric and positional fatty acid (FA), fatty acid methyl ester (FAME), diacylglycerol (DAG) and triacylglycerol (TAG) isomers. Discovery Ag-Ion SPE is shown in this application to separate FAMEs from an edible oil sample.

Legal Information

Discovery is a registered trademark of Merck KGaA, Darmstadt, Germany
SP is a registered trademark of Sigma-Aldrich Co. LLC

Analytical column

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SPE tube or plate

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