Citation: SHAO Shiping, XIANG Dapeng, LI Shuang, XI Xinglin, CHEN Wenrui. Determination of docosahexaenoic acid in milk powder by gas chromatography using acid hydrolysis[J]. Chinese Journal of Chromatography, ;2015, 33(11): 1214-1218. doi: 10.3724/SP.J.1123.2015.06022 shu

Determination of docosahexaenoic acid in milk powder by gas chromatography using acid hydrolysis

1.
Inspection and Quarantine Technology Centre, Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China

Corresponding author: SHAO Shiping,
Received Date: 17 June 2015

Fund Project: 广东省广州市科技计划项目(12S496140081). (12S496140081)

A method to determine docosahexenoic acid (DHA) in milk powder by gas chromatography was established. The milk powder samples were hydrolyzed with hydrochloric acid, extracted to get total fatty acids by Soxhlet extractor, then esterified with potassium hydroxide methanol solution to form methyl esters, and treated with sodium hydrogen sulfate. The optimal experiment conditions were obtained from orthogonal experiment L₉(3³) which performed with three factors and three levels, and it requires the reaction performed with 1 mol/L potassium hydroxide solution at 25 ℃ for 5 min. The derivative treated with sodium hydrogen sulfate was separated on a column of SP-2560 (100 m×0.25mm×0.20 μ m), and determined in 55 min by temperature programming-gas chromatography. Good linearity was obtained in the range 5.0-300 mg/L with the correlation coefficient of 0.9999. The relative standard deviations (RSDs) were 3.4%, 1.2% and 1.1% for the seven repeated experiments of 10, 50 and 100 mg/L of DHA, respectively. The limit of detection was 2 mg/kg, and the recoveries of DHA were in the range of 90.4%-93.5%. The results are satisfactory through the tests of practical samples.
- gas chromatography (GC),
- docosahexenoic acid (DHA),
- milk powder,
- acid hydrolysis
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沈阳化工大学材料科学与工程学院沈阳 110142