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食品中维生素K1、甲萘醌-4和甲萘醌-7的测定

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文章建立一种同时测定食品中维生素K1、甲萘醌-4(Menaquinone-4,MK-4)和甲萘醌-7(Menaquinone-7,MK-7)含量的方法,以评估不同食品中维生素K的含量.样品经酶解、正己烷提取后,采用液相色谱串联质谱法进行分析.采用Agilent Poroshell 120 EC-C18色谱柱(50 mmx3.0 mm,2.7 μm)进行分离,以0.1%甲酸乙腈-0.1%甲酸甲醇为流动相梯度洗脱.采用大气压化学电离源,正离子模式,选择反应监测模式检测.通过对色谱条件优化,在4 min内实现了3种维生素K的测定.维生素K1、MK-4和MK-7在0.5~500.0ng/mL浓度范围内线性良好,相关系数r2>0.9932;加标回收率在87.5%~110.7%,相对标准偏差<7.09%.将该方法应用于27种食品中维生素K含量的测定,蔬菜类食品中维生素K1的含量较高,肉蛋类食品中以MK-4为主,MK-7在发酵豆制品中含量较高.该方法操作简单、重现性好、准确度高,适用于食品中维生素K1、MK-4和MK-7的含量测定,可为维生素K膳食摄入提供参考.
Determination of Vitamin K1,Menaquinone-4 and Menaquinone-7 in Food
A method for simultaneous determination of vitamin K1,menaquinone-4(MK-4)and menaquinone-7(MK-7)content in food was established,and to evaluate the levels of vitamin K in different foods.After enzymatic hydrolysis and n-hexane extraction,food samples were analyzed by liquid chromatography-tandem mass spectrometry.The chromatographic separation was carried out on an Agilent Poroshell 120 EC-C18 column(50 mm×3.0 mm,2.7 μm),with 0.1% formic acid acetonitrile and 0.1% formic acid methanol as mobile phase gradient elution.Mass spectrometry method was carried out with atmospheric pressure chemical ionization source,multiple reaction monitoring mode for positive ion detection.Under the optimum conditions,vitamin K1,MK-4 and MK-7 were determined within 4 min.All analytes achieved good linearity in the range of 0.5-500.0 ng/mL,with correlation coefficient higher than 0.9932.The recoveries rates of standard addition were between 87.5% and 110.7%,with the relative standard deviations less than 7.09%.The method was applied to determine the content of vitamin K in 27 kinds of food,the content of vitamin K1 was higher in vegetable foods,MK-4 was the main vitamin K in meat and eggs,and MK-7 was higher in fermented soybean products.The method was simple,reproducible and accurate,and was suitable for the determination of vitamin K1,MK-4 and MK-7 in food.

vitamin K1menaquinone-4menaquinone-7foodliquid chromatography-tandem mass spectrometry

贾永娟、刘杏立、刘春冉、赵金宝、倪君君

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北京和合医学诊断技术股份有限公司研究院,北京 100011

维生素K1 甲萘醌-4 甲萘醌-7 食品 液相色谱-串联质谱法

2024

食品科技
北京市粮食科学研究所

食品科技

CSTPCD北大核心
影响因子:0.622
ISSN:1005-9989
年,卷(期):2024.49(1)
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