Comparison of the methylation methods for the determination of fatty acids in Yak bones by gas chromatography

doi:10.3724/SP.J.1123.2016.07009

Abstract

Abstract:

The acid hydrolysis-esterification system with six methylation methods (acetyl chloride-methanol method, H₂SO₄-methanol method, HCl-methanol method, KOH-methanol method, KOH-methanol+H₂SO₄-methanol method and KOH-methanol+HCl-methanol method) were compared for the fatty acids (FAs) profiling of Yak bones by gas chromatography (GC) in this study. Good linearities were obtained in the range of 0.28-250.00 mg/L with correlation coefficient R²>0.99, except for C4:0 (R²=0.9878). FAs can hardly be detected by the base-catalytic method and the combined acid-base method (the content of total FAs was less than 0.20 g/100 g) in the present study. The FAs determined by the acetyl chloride-methanol method (content of total FAs was 13.61 g/100 g) was superior to the H₂SO₄-methanol method (content of total FAs was 11.68 g/100 g) and the HCl-methanol method (content of total FAs was 3.18 g/100 g). The precisions for intra-day and inter-day of acetyl chloride-methanol method and H₂SO₄-methanol method were 0.27%-8.60% and 0.34%-2.64%, respectively. And the recoveries for the FAs of these two methods were in the range of 83.06%-105.54%. This study suggested that the acid hydrolysis-acetyl chloride-methanol method was the best method in the six methods. It was convenient for the accurate determination of FAs in Yak bones. C18: 1n9c, C16: 0, C18: 0 and conjugated linoleic acid (CLA) were the mainly FAs in Yak bones, and the sum of the four FAs was more than 85% of the total FAs. The ratio of the contents of the saturated and unsaturated FAs in Yak bones was about 1: 2. The study of fatty acids in Yak bones provides an important basis for the effective utilization of bone resources.

Key words: fatty acids, gas chromatography (GC), method validation, methylation, Yak bones

CLC Number:

O658

LIU Wenyuan, JIA Wei, WU Ting, ZHANG Chunhui, LI Xia, CHEN Xuefeng. Comparison of the methylation methods for the determination of fatty acids in Yak bones by gas chromatography[J]. Chinese Journal of Chromatography, 2016, 34(11): 1113-1119.

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