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高效液相色谱法测定乳粉中VK2(七烯甲萘醌)含量 被引量:3

Determination of Vitamin K2 (Menaquinone-7) in Milk Powder by High Performance Liquid Chromatography
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摘要 建立使用高效液相色谱快速检测乳粉中VK2(七烯甲萘醌(menaquinone-7,MK-7))含量的方法。乳粉样品用250 mg/g脂肪酶酶解2 h,经500 mg/g碳酸钾皂化,正己烷提取,旋转蒸发浓缩,甲醇-异丙醇(4∶1,V/V)复溶,用C18色谱柱及还原柱柱后衍生,经高效液相色谱-荧光检测器测定,外标法定量。结果表明:MK-7在19.47 min附近出峰,标准曲线在MK-7质量浓度0.0~1.5μg/mL范围内呈良好线性关系(R^2=0.99995);空白乳粉样品中MK-7添加量为5、10、25μg/100 g时,加标回收率为87.9%~94.3%,相对标准偏差为0.9%~6.4%;取样量为2 g、定容体积为1 mL时,MK-7检测限为0.15μg/100 g,定量限为0.5μg/100 g。本检测方法前处理简单,具有较高准确度、灵敏度和稳定性,可以用于乳粉中VK2(MK-7)含量的检测。 This paper describes a method for determination of vitamin K2(menaquinone-7,MK-7)in milk powder using high performance liquid chromatography(HPLC).The sample was hydrolyzed with lipase(250 mg/g)for 2 h,saponified with potassium carbonate(500 mg/g),extracted with n-hexane,concentrated by rotary evaporation,reconstituted with methanol/isopropanol(4:1),and post-derivatized with C18 column and reduced column before being analyzed by HPLC with a fluorescence detector.The analyte was quantified by external standard method.The results showed that the peak of MK-7 appeared at about 19.47 min,and the calibration curve for it showed a good linear relationship in the range of 0.0–1.5μg/mL(R^2=0.99995).The recoveries for blank samples spiked at 5,10 and 25μg/100 g were between 87.9%and 94.3%,with relative standard deviations of 0.9%–6.4%.When 2 g of sample was taken and the volume was made up to 1 mL,the detection limit was 0.15μg/100 g and the quantification limit was 0.5μg/100 g.The method was simple with high accuracy,sensitivity and stability,and could be used for the detection of vitamin K2(MK-7)content in milk powder.
作者 王瑶 张敏 马晓冲 刘星 柴艳兵 张耀广 李飞 李兴佳 WANG Yao;ZHANG Min;MA Xiaochong;LIU Xing;CHAI Yanbing;ZHANG Yaoguang;LI Fei;LI Xingjia(Quality Management Center of Junlebao Dairy Group,Shijiazhuang 050021,China)
出处 《乳业科学与技术》 2019年第6期30-33,共4页 JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY
关键词 乳粉 VK2 七烯甲萘醌 高效液相色谱 荧光检测器 定量测定 milk powder vitamin K2 menaquinone-7 high performance liquid chromatography fluorescence detector quantitative determination
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