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乳业科学与技术 ›› 2019, Vol. 42 ›› Issue (6): 30-33.DOI: 10.15922/j.cnki.jdst.2019.06.006

• 分析检测 • 上一篇    下一篇

高效液相色谱法测定乳粉中VK2（七烯甲萘醌）含量

王瑶, 张敏, 马晓冲, 刘星, 柴艳兵, 张耀广, 李飞, 李兴佳   

  1. 君乐宝乳业集团质量管理中心, 河北石家庄, 050021
  • 出版日期:2019-11-01 发布日期:2021-11-09

Determination of Vitamin K2 (Menaquinone-7) in Milk Powder by High Performance Liquid Chromatography

WANG Yao, ZHANG Min, MA Xiaochong, LIU Xing, CHAI Yanbing, ZHANG Yaoguang, LI Fei, LI Xingjia   

  1. (Quality Management Center of Junlebao Dairy Group, Shijiazhuang 050021, China)
  • Online:2019-11-01 Published:2021-11-09

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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0.0～1.5 μg/mL范围内呈良好线性关系（R2=0.999 95）；空 白乳粉样品中MK-7添加量为5、10、25 μg/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0.15 μg/100 g，定量限为0.5 μg/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。

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

Abstract: 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 0.0–1.5 μg/mL (R2 = 0.999 95). The recoveries for blank samples spiked at 5, 10 and 25 μg/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 0.15 μg/100 g and the quantification limit was 0.5 μg/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.

Key words: milk powder; vitamin K2; menaquinone-7; high performance liquid chromatography; fluorescence detector; quantitative determination

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