孙晓菲,章秀梅,高玉静,邱洁,刘欣,李帅,张琨.高效液相色谱荧光法测定营养素补充制剂中维生素K2(MK-7)的含量[J].,2020,36(6):321-327.
高效液相色谱荧光法测定营养素补充制剂中维生素K2(MK-7)的含量
Determination of Vitamin K2 (MK-7) in Nutrient Supplements by High Performance Liquid Chromatography-Fluorescence Spectrometry
投稿时间:2019-12-09  
DOI:10.13982/j.mfst.1673-9078.2020.6.1209
中文关键词:  维生素K2  高效液相色谱法  衍生  荧光
英文关键词:Vitamin K2 (MK-7)  high performance liquid chromatography (HPLC)  derive  fluorescence
作者简介:孙晓菲,(1990-),女,助理工程师,研究方向:营养、保健食品的分析检测 通讯作者:张琨,(1981-),男,高级工程师,研究方向:营养、保健食品的研究开发
基金项目:湖北省博士后创新岗位(鄂博管办[2016]5号)
作者单位
孙晓菲 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
章秀梅 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
高玉静 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
邱洁 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
刘欣 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
李帅 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
张琨 (福格森(武汉)生物科技股份有限公司,湖北武汉 430056) 
AuthorInstitution
SUN Xiao-fei (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
ZHANG Xiu-mei (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
GAO Yu-jing (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
QIU Jie (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
LIU Xin (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
LI Shuai (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
ZHANG Kun (Ferguson (Wuhan) Biotechnologies Co. Ltd., Wuhan 430056, China) 
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中文摘要:
      建立高效液相色谱荧光法(HPLC-FLD)测定营养素补充制剂中维生素K2(MK-7)的含量。样品用异丙醇超声提取30 min,提取液离心过滤后取样液10 μL注入液相色谱系统中。样液经安捷伦C18色谱柱(4.6 mm×150 mm,5 μm)或其他等效色谱柱分离,柱后采用锌粉还原柱(4.6 mm×50 mm)衍生,使样品中维生素K2(MK-7)具有荧光特性。以甲醇(含5%四氢呋喃,冰乙酸0.03%,乙酸锌1.0 g/L)为流动相,流速1.0 mL/min,检测波长 激发波长243 nm发射波长430 nm。当称取样品1.0 g,定容体积为10 mL时,MK-7的检出限为0.03 μg/g,定量限为0.1 μg/g;MK-7在浓度0~2.176 μg/mL的范围内线性关系良好,线性相关系数为R2=0.9999;重复性实验中RSD%为0.97%;样品加标回收率为93.40%。此方法操作简单,高效,准确,重现性好,可用于营养素补充制剂中维生素K2(MK-7)的含量测定。
英文摘要:
      To establish a method for the determination of Vitamin K2 (MK-7) in Nutrient Supplements by high performance liquid chromatography-fluorescence detector (HPLC-FLD), the sample was extracted by isopropanol ultrasonic for 30 min, after centrifugation and filtration, 10 μL of the sample solution was injected into the liquid chromatography system. The sample solution was separated by Agilent C18 column (4.6 mm×150 mm, 5 μm) or equivalent column. After the column, it was derived by zinc powder reduction column (4.6 mm×50 mm), so that the Vitamin K2 (MK-7) in the sample had fluorescence characteristics. Methanol (containing 5% tetrahydrofuran, glacial acetic acid 0.03%, zinc acetate 1.0 g/L) was used as mobile phase, the flow rate was 1.0 mL/min, the fluorescence detector was set at λex/λem=243 nm/430 nm. When the sample weight was 1.0 g and the volume was 10 mL, the detection limit of this method was 0.03 μg/g, and the quantitative limit was 0.1 μg/g, MK-7 had a good linearity in the range of 0~2.176 μg/mL, the R2 was 0.9999. The relative standard deviation of the repeatability experiment was 0.97%, and the recovery of the standard was 93.40%. This method has simple operation, good accuracy, and good reproducibility. It can be used for the determination of MK-7 in Nutrient supplements.
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