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Zeng Y.,Guangzhou Wine Analytical Center | Ding Y.,Guangzhou Wine Analytical Center
Modern Food Science and Technology | Year: 2013

In this paper, through four factors such as temperature, time, the ratio of gas-liquid phase and salting out, the determination of methanol in wine by head space GC with capillary column was studied and the optimal conditions were found as following: using a Phenomenex ZB-WAX chromatographic column and a FID detector. The split ratio was 20 with split liner tube (2 mm I. D) and the flow rate of carrier gas was 2.0 mL/min. The heated temperature was 70°C with head space sampling used and vial equilibration time was 15 min and sample volume was 5 mL in a 20 mL vial. The linear of this method was satisfied when the concentration of methanol was at the range of 10.2~407.6 mg/L (r=0.9997). The lowest method detection limit was 8.5 mg/L and the average recovery rate was 99.2%. RSD of Repeat was 1.4%. It was shown that this method is more simple and efficient than GC method in GB/T15038-2006, and the result was reliable.


Zeng Y.,Guangzhou Wine Analytical Center | Ding Y.,Guangzhou Wine Analytical Center | Peng C.,Guangzhou Wine Analytical Center | Peng C.,South China University of Technology
Modern Food Science and Technology | Year: 2014

In this paper, 3 mL wine was diluted with water (7 mL) and internal standard solution (60 μL 0.02% (V/V) 4-Methyl-2-pentanol), salted with 4.5 g ammonium sulfate and then extracted with 0.5 mL dichloromethane. After scrolled for 10 min and centrifuged for 10 min, the extract was injected in a GC system. ZB-WAX capillary column (30 m × 0.25 mm × 0.25 μm) used with the temperature program was as follows: 40°C for 5 min, then raised at 3°C/min up to 190°C for 10 min. N2 was used as carrier gas with flow rate of 1.5 mL/min, injection volume and input temperature were 0.5 mL and 200°C, and the injection mode was splitless. The results were detected by FID. The method could isolate 63 compounds from wine, and 30 of them were analyzed qualitatively. They included nine alcohols, eleven esters, eight organic acids, two aldoketones. Repeatability of 28 of them was less than 10% (as RSD) with the recoveries from 85% to 120%. The quantitative analysis by using internal standard solution was accurate. This method has the advantages of simple operation, little pollution, short time of pretreatment and good repeatability and accuracy, which satisfies the further demand of wine fingerprinting analysis technology.

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