1 H NMR Quantification of DHA and EPA in Fish Oil
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H NMR Quantification of DHA and EPA in Fish Oil
LV Jinxiao1), #, WANG Cong1), 2), 3), 4), #, ZHANG Xiuli1), 2), 3), 4), LV Zhihua1), 2), 3), 4), *, and YU Mingming1), 2), 3), 4), * 1) School of Medicine and Pharmacy, Ocean University of China, Qingdao 266003, China 2) Laboratory for Marine Drugs and Bioproducts of Qingdao National Laboratory for Marine Science and Technology, Qingdao 266003, China 3) Key Laboratory of Glycoscience & Glycotechnology of Shandong Province, Qingdao 266003, China 4) Key Laboratory of Marine Drugs, Ministry of Education of China, Qingdao 266003, China (Received December 2, 2019; revised April 28, 2020; accepted May 3, 2020) © Ocean University of China, Science Press and Springer-Verlag GmbH Germany 2020 Abstract Fish oil is a popular nutritional product consumed in China. The beneficial effects of fish oil have been attributed to docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA). Hence, it is crucial to develop a rapid and precise method to determine the contents of EPA and DHA in fish oil. In this study, a rapid and accurate proton nuclear magnetic resonance method for the quantification of DHA and EPA was developed. Dimethyl terephthalate was selected as an internal standard, and the signals at 2.391 ppm for DHA and at 1.697 ppm for EPA were chosen for the quantification. Validation of the method was performed in terms of specificity, precision, and stability. The results indicated that the method was precise and in line with the China Food and Drug Administration guidance. The method has been successfully applied to characterize fish oil capsules obtained from four pharmaceutical companies. This study indicated that the rapid 1H NMR method is suitable for the quality control of fish oil. Key words
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H NMR; EPA; DHA; fish oil; quality control
1 Introduction Fish oil is the oil derived from marine pelagic fish species, such as tuna, salmon, swordfish, and mackerel (Jacobs et al., 2002; Smith and Sahyoun, 2005). Fish oil exerts some beneficial effects against several diseases such as autoimmune disease (Harbige, 2003), cardiovascular diseases (Kris-Etherton et al., 2002), depression (Nemets et al., 2006), and neurological disorders (Lukiw and Bazan, 2008). The beneficial effects of fish oil have been attributed to docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA) (Fig.1) which have been associated with these health benefits. As a result, there are numerous fish oil products containing EPA and DHA in the markets. These fish oil products are derived from different sources, and the prices of these products are significantly different. While these products are labeled with the same ingredient levels, namely DHA (120 mg g−1) and EPA (180 mg g−1) (Yi et al., 2014). The quantitative methods of DHA and EPA in fish oil products have been developed by gas chromatography (GC) (Srigley and Rader, 2014), gas chromatography-mass spectrometry (GC-MS) (Yi et al., 2014), and # The two authors contributed equally to the work. * Corresponding authors. E-mail: [email protected] E-
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