This study aims to develop a method for simultaneous determination of some monoglyceride (MG) and diglyceride (DG) emulsifiers including: monoolein (MO), monostearin (MS), monopalmitin (MP), dipalmitin (DP) in milk by liquid chromatography-mass spectrometry. The sample was ultrasonically extracted with a solvent mixture of chloroform: methanol (MeOH) in the ratio of 2:1 at 45℃ for 30 minutes. The extract was evaporated, dissolved with MeOH and analyzed on a liquid chromatography-mass spectrometry system with the following conditions: C18 chromatography column (2.1 mm x 150 mm; 3.5 µm), mobile phase was 100% MeOH, flow rate was 0.3 mL/min, MS detector was in atmospheric pressure chemical ionization mode (APCI). The method had good specificity, the standard curve had a coefficient of R2 ≥ 0.9995. The repeatability was in the range of 2.54 - 7.21%, the recovery was in the range of 80.4 -99.5%, the limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.6 mg/kg and 0.2 mg/kg for MO, MP, MS, respectively; 0.15 mg/kg and 0.5 mg/kg for DP. The method was applied to analyze the emulsifiers in 20 different milk samples collected in Hanoi. The total content of 04 emulsifiers ranged from 4.51 - 42.2 mg/kg for powder milk and 4.67 - 12.6 mg/kg for liquid milk.
Monoglyceride, diglyceride, milk, liquid chromatography-mass spectrometry.
[1]. Abdul Rohman, Yaakob B, Che Man and Eka Noviana, "Analysis of Emulsifier in Food Using Chromatographic Techniques,” Journal of Food and Pharmaceutical Sciences, no 1, pp. 54-59, 2013.
[2]. G. L. Hasenhuettl, R. W. Hartel (eds.), Food Emulsifiers and Their Applications, Second Edition, Springer Nature Switzerland AG, 2019.
[3]. Shane N.D. Lal, Charmian J. O'Connor, Laurence Eyres, "Application of emulsifiers/stabilizers in dairy products of high rheology,” Advances in Colloid and Interface Science, 123–126, pp.433–437, 2006.
[4]. Circular 24/2019/TT-BYT. Circular on management and use of food additives [in Vietnamese].
[5]. Panyod S., Wu W.-K., Chang C.-T., Wada N., et al., "Common dietary emulsifiers promote metabolic disorders and intestinal microbiota dysbiosis in mice," Communications Biology, vol 7, 1:749, 2024.
[6]. Claudia Oellig, Klara Brändle, Wolfgang Schwack, "Characterization of E 471 food emulsifiers by high-performancethin-layer chromatography–fluorescence detection," Journal of Chromatography A, 2018.
[7]. Bruno Marcato, "Giuliano Cecchin. Analysis of mixtures containing free fatty acids and mono, di and triglycerides by high-performance liquid chromatography coupled with evaporative light-scattering detection," Journal of Chromatography A, vol 730, pp. 83-90, 1996.
[8]. Liu, T. Lee, E. Bobik, Jr., M. Guzman-Harty and C. Hastilow, "Quantitative Determination of Monoglycerides and Diglycerides by High-Performance Liquid Chromatography and Evaporative Light-Scattering Detection," Journal of the American Oil Chemists' Society, vol. 70, no. 4, 1993.
[9]. A. Lopez-Lopez, A.I. Castellote-Bargallo, M.C. Lopez-Sabater, "Direct determination by high-performance liquid chromatography of sn-2 monopalmitin after enzymatic lipase hydrolysis," Journal of Chromatography B, vol. 760, pp. 97–105, 2001.
[10]. T. Riist. Riisom and L. Hoffmeyer OM, "High Performance Liquid Chromatography Analyses of. Emulsifiers: I. Quantitative Determinations of Mono- and Diacylglycerols of Saturated Fatty Acids," Journal of the American oil chemist’s societ, vol 55, pp 649-652, 1978.
[11]. Bareth A., Strohmar W., Kitzelmann E., "Gas chromatographic determination of mono-and diglycerides in milk and milk products," European Food Research and Technology, vol 216, no4, pp.365-368, 2003.
[12]. Chiemi Satou, Hirofumi Goto, Yuya Yamazaki, Katsuyoshi Saitou, Shoji Matsumoto, Ou Takahashi, Yosuke Miyazaki, Keiichi Ikuta and Yosuke Yajima, "Modified Gas Chromatographic Method to Determine Monoacylglycerol and Diacylglycerol Contents in Edible Fats and Oils,” Journal of Oleo Science, vol 66, no.6, pp.601-606, 2017.
[13]. Suman M., Silva G., Catellani D., Bersellini U., et al., "Determination of food emulsifiers in commercial additives and food products by liquid chromatography/atmospheric-pressure chemical ionisation mass spectrometry," Journal of Chromatography A, vol. 1216, no. 18, pp.3758-3766, 2009.
[14]. Marcato B., Cecchin G., "Analysis of mixtures containing free fatty acids and mono-, di-and triglycerides by high-performance liquid chromatography coupled with evaporative light-scattering detection," Journal of Chromatography A, vol. 730, no.1-2, pp.83-90, 1996.
[15]. Dinah Schick, Katharina Link, Wolfgang Schwack, Michael Granvog Claudia Oellig, "Analysis of mono , di , triacylglycerols, and fatty acids in food emulsifiers by high performance liquid chromatography–mass spectrometry," European Food Research and Technology, no.247, pp.1023–1034, 2021.
[16]. Flor R. V., Prager M. J., "Lipid extraction procedure for some food products containing surfactants," Journal of the Association of Official Analytical Chemists, vol. 63, no. 1, pp.22-26, 1980.
[17]. Chu B.-S., Nagy K., "Enrichment and quantification of monoacylglycerols and free fatty acids by solid phase extraction and liquid chromatography–mass spectrometry," Journal of Chromatography B, vol. 932, pp.50-58, 2013.
[18]. La Nasa J., Degano I., Brandolini L., Modugno F., et al., "A novel HPLC-ESI-Q-ToF approach for the determination of fatty acids and acylglycerols in food samples," Analytica chimica acta, vol. 1013, pp.98-109, 2018.
[19]. Tran Cao Son, Le Thi Hong Hao et al., Method validation and evaluation of measurement uncertainty in chemical analysis, Science and Technology Publishing, 2021 [In Vietnamese].