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柱后还原-高效液相色谱法测定调制乳粉中维生素K及维生素K

[Determination of vitamin K and vitamin K in modulation milk powder by post-column reduction-high performance liquid chromatography].

作者信息

Sun Shanshan, Gong Pixue, Zhang Yanxia, Wang Mingdong, Lu Lanxiang, Li Xinling, Xue Xia, Liu Yanming, Zhang Feng

机构信息

Shandong Institute for Food and Drug Control, Ji'nan 250101, China.

Chinese Academy of Inspection and Quarantine, Beijing 100176, China.

出版信息

Se Pu. 2020 Jul 8;38(7):847-852. doi: 10.3724/SP.J.1123.2019.11020.

Abstract

A method for the determination of vitamin K and vitamin K 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 -hexane, and dissolved in methanol after concentration. The vitamin K were first separated on an Xbridge C 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 K and vitamin K 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 K and vitamin K were 0.07 μg/100 g and 0.2 μg/100 g, respectively. The limits of quantification of vitamin K and vitamin K 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 K and vitamin K in formula milk powder.

摘要

建立了一种采用高效液相色谱(HPLC)柱后还原法测定调制乳粉中维生素K和维生素K的方法。样品用水溶解,经脂肪酶水解,用2.5mol/L氢氧化钠溶液和乙醇溶液皂化,用正己烷萃取,浓缩后溶于甲醇。维生素K先在Xbridge C柱上分离,再在锌粉还原柱上分离,用荧光检测器检测。激发波长和发射波长分别为326nm和432nm。采用外标法定量。结果表明,维生素K和维生素K的线性范围分别为0.0025 - 2.0μg/mL和0.01 - 2.0μg/mL,相关系数均大于0.999。加标回收率为80.39% - 94.39%,精密度为0.85% - 3.98%。维生素K和维生素K的检出限分别为0.07μg/100g和0.2μg/100g。维生素K和维生素K的定量限分别为0.2μg/100g和0.8μg/100g。该方法灵敏度高、重复性好,结果准确。适用于配方乳粉中维生素K和维生素K的分析测定。

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