Citation: SUN Shanshan, GONG Pixue, ZHANG Yanxia, WANG Mingdong, LU Lanxiang, LI Xinling, XUE Xia, LIU Yanming, ZHANG Feng. Determination of vitamin K₁ and vitamin K₂ in modulation milk powder by post-column reduction-high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2020, 38(7): 847-852. doi: 10.3724/SP.J.1123.2019.11020 shu

Determination of vitamin K₁ and vitamin K₂ in modulation milk powder by post-column reduction-high performance liquid chromatography

1.
Shandong Institute for Food and Drug Control, Ji'nan 250101, China;
2.
Chinese Academy of Inspection and Quarantine, Beijing 100176, China

Corresponding author: LIU Yanming, ZHANG Feng,
Received Date: 22 November 2019

Fund Project: Shandong Keypoint Research and Invention Program (Food for Special Medical Purpose, FSMP) (No. 2019YYSP020)

A method for the determination of vitamin K₁ and vitamin K₂ in modulation milk powder was developed by high performance liquid chromatography (HPLC) coupled with post-column reduction. The samples were dissolved in water, lipase hydrolyzed, saponified with 2.5 mol/L sodium hydroxide solution and ethanol solution, extracted with n-hexane, and dissolved in methanol after concentration. The vitamin K were first separated on an Xbridge C₁₈ column and then on a zinc powder reduction column, and detected using a fluorescence detector. The excitation and emission wavelengths were 326 nm and 432 nm, respectively. An external standard method was used for quantification. The results showed that the linearities of vitamin K₁ and vitamin K₂ was in the ranges of 0.0025-2.0 μg/mL and 0.01-2.0 μg/mL, respectively, with correlation coefficients both greater than 0.999. The spiked recoveries were 80.39%-94.39% and the precisions were 0.85%-3.98%. The limits of detection of vitamin K₁ and vitamin K₂ were 0.07 μg/100 g and 0.2 μg/100 g, respectively. The limits of quantification of vitamin K₁ and vitamin K₂ were 0.2 μg/100 g and 0.8 μg/100 g, respectively. The method has high sensitivity and good repeatability, and gives accurate results. It is suitable for the analysis and determination of the vitamin K₁ and vitamin K₂ in formula milk powder.
- high performance liquid chromatography (HPLC),
- fluorescence detector,
- post-column reduction,
- vitamin K₁,
- vitamin K₂,
- modulation milk powder
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沈阳化工大学材料科学与工程学院沈阳 110142

Determination of vitamin K1 and vitamin K2 in modulation milk powder by post-column reduction-high performance liquid chromatography

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通讯作者: 陈斌, bchen63@163.com

Determination of vitamin K₁ and vitamin K₂ in modulation milk powder by post-column reduction-high performance liquid chromatography