G003760

GC Analysis of FAMEs in Popcorn Oil on SP^®-2560 (75 m x 0.18 mm I.D., 0.14 μm) after SPE Fractionation using Discovery^® Ag-Ion, Fast GC Analysis

application for SPE, suitable for GC

Properties

• 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

Description

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