[Objective]An analytical method for the simultaneous determination of vitamin K1 and K2 in dairy products by high performance liquid chromatography-fluorescence detector was established.[Method]The samples were hydrolyzed by lipase,extracted with n-hexane after saponification,derivatized by zinc powder reduction column,determined by high performance liquid chromatography-fluorescence detector and quantified by external standard method.[Result]Peaks of vitamin K1 and K2 were separated within 15 mins.The linear range was good in the concentration of 0.1~1.6 μg/mL,and the correlation coefficient was ≥0.99.When the sample volume was 5 g and the constant volume was 5 mL,the detection limit of vitamin K1 and K2 was 2 μg/100g,and the quantitation limit was 6 μg/100g.When the addition amount was 5~50 μg/100g,the recovery rate of vitamin K1 was 61.0% to 108.5%,the precision RSD was 1.1% to 9.3%,the recovery rate of vitamin K2 was 75.6% to 104.0%,and the RSD was 2.0% to 6.6%,which met the requirements of precision and recovery.[Conclusion]The established method had good recovery rate,high accuracy and good repeatability,and could detect the content of vitamin K1 and K2 in dairy products.
LI Huijuan
. Simultaneous Determination of Vitamin K1 and K2 in Dairy Products[J]. China Dairy, 2024
, 0(9)
: 68
-72
.
DOI: 10.12377/1671-4393.24.09.12
[1] Dam H.The antihmorrhagic vitamin of the chick:Occurrence and chemical nature[J].Nature,1935,135(3417):652-653.
[2] 刘黎明,帖利军,史晓薇,等.维生素K与儿童健康关系的研究[J].中国妇幼健康研究,2019,30(9):1039-1047.
[3] Shea M,Sarah B.Concepts and controversies in evaluating vitamin K status in population-based studies[J].Nutrients,2016,8(1):8.
[4] Halder M,Petsophonsakul P,Akbulut A C,et al.Vitamin K:Double bonds beyond coagulation insights into differences between vitamin K1 and K2 in health and disease[J].International journal of molecular sciences,2019,20(4):896.
[5] 于翰宗,田蒙,姜山,等.高效液相色谱-荧光检测法测定大白菜中维生素K1含量[J].湖北农业科学,2022,61(20):149-152.
[6] 邹连蓬,张雪松,黄百芬,等.动物性食物不同形式维生素K检测方法的建立[J].卫生研究,2019,48(3):468-473.
[7] 聂淑慧,胡贻椿,段一凡,等.国内外维生素K研究现状及膳食参考摄入量修订进展[J].营养学报,2022,44(2):105-111.
[8] 邓梦雅,彭祖茂,朱丽,等.高效液相色谱–荧光检测法测定食品中维生素K2的含量[J].食品工业科技,2019,40(19):240-244,250.
[9] 刘琳,吕宁,林超等.乳及乳制品中维生素K2的发展现状及展望[J].中国乳业,2023(6):79-84.
[10] 毛新武,黄景初,何淑明,等.在线固相萃取-高效液相色谱法快速测定奶粉中的维生素K1与维生素K2[J].食品安全质量检测学报,2022,13(16):5305-5313.
[11] 王瑶,张敏,马晓冲,等.高效液相色谱法测定乳粉中VK2(七烯甲萘醌)含量[J].乳业科学与技术[J].2019,42(6):30-33.
[12] 林国斌,华永有,倪蕾,等.高效液相色谱法测定保健食品功效成分七烯甲萘醌含量[J].海峡预防医学杂志,2022,28(2):4-6.
[13] 许强,孟凡达,王轶鹏,等.高效液相色谱–荧光检测法测定保健食品中的维生素K1和维生素K2[J].理化检验(化学分册),2021,57(7):618-620.
[14] 刘光兰,郑良,吴银,等.高效液相色谱法同时测定维生素D3和维生素K2的含量[J].食品安全质量检测学报,2019,10(5):1225-1229.
[15] Manoury E,Jourdon K,Boyaval P,et al.Quantitative measurement of vitamin K2(menaquinones) in various fermented dairy products using a reliable high-performance liquid chromatography method[J].Journal of Dairy Science,2013,96(3):1335-1346.
[16] 赵彦远,温敏辉,黄正华.奶粉中维生素K2检测方法的研究[J].现代信息科技,2022,6(10):161-164.
[17] 梁红艳,温洁,姜晓峰.利用毛细管电泳测定血清中维生素K的含量[J].中国实验诊断学,2003,7(2):87-89.
[18] 王聪,梁瑞强,曹进,等.液相色谱-质谱联用法测定保健食品9 种脂溶性维生素[J].食品安全质量检测学报,2016,7(3):991-999.
[19] 全思思. 超高效液相色谱/超临界流体色谱-串联质谱联用技术同时测定婴幼儿配方乳粉中多种维生素的研究[D].广州:广东药学院,2017.
[20] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 27404—2008 实验室质量控制规范食品理化检测[S].
[21] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 27417—2017 合格评定化学分析方法确认和验证指南[S].
