摘要
建立高效液相色谱法测定保健食品中七烯甲萘醌(MK-7)。含油脂类食品先经脂肪酶酶解,再经异丙醇提取,不含油食品直接使用异丙醇超声提取,采用高效液相紫外检测器进行检测。用Intersil ODS–3 C_(18)型色谱柱(4.6 mm×150 mm,5μm),以甲醇–异丙醇(体积比为75∶25)为流动相,流量为1.0 mL/min,检测波长为270 nm,柱温为40℃,进样体积为20μL。MK-7的质量浓度在0.4-20 mg/L的范围内与色谱峰面积具有良好的线性关系,相关系数为0.9998,方法检出限为0.06 mg/L,定量限为0.2 mg/L。含油脂类食品与不含油脂类食品中MK-7平均加标回收率分别为96.2%、103.2%,测定结果的相对标准偏差分别为0.9%、1.0%(n=9)。室温下,MK-7样品溶液在24 h内稳定。该方法操作简单,可用于保健食品中MK-7的含量测定。
A method was developed for the determination of menatetrenone 7(MK-7)in health food by high performance liquid chromatography(HPLC).Oily foods were first hydrolyzed by lipase and then extracted by isopropyl alcohol.Oil-free foods were directly extracted by isopropyl alcohol ultrasonic and detected by high performance liquid phase with an ultraviolet detector.An Intersil ODS–3 C_(18) column(4.6 mm×150 mm,5μm)was employed at the column tempereture of 40℃.The mobile phase consisted of methanol–isopropyl alcohol(volume ratio was 75∶25)was at the flow rate of 1.0 mL/min.The detection wavelength was 270 nm and the injection volume was 20μL.The mass concentration of MK-7 had a good linear relationship with the chromatographic peak area in the range of 0.4–20 mg/L with the correlation coefficients of 0.9998.The limit of detection(LOD)of the method was 0.06 mg/L.The limit of quantitation(LOQ)was 0.2 mg/L.The average recovery rates of oily foods and oil-free foods were 96.2%and 103.2%,respectively,with the relative standard deviations of measurement results were 0.9%and 1.0%,respectively(n=9).MK-7 solution was stable in 24 h at room temperature.This developed method has simple operation,and it can be widely applied to determine content of MK-7 in health foods.
作者
程岁寒
覃先武
朱金玲
潘存锋
张海波
张彦
Cheng Suihan;Qin Xianwu;Zhu Jinling;Pan Cunfeng;Zhang Haibo;Zhang Yan(The Hubei Provincial Key Laboratory of Yeast Function,Angel Nutritech Co.,Ltd.,Yichang 443003,China)
出处
《化学分析计量》
CAS
2021年第12期69-73,共5页
Chemical Analysis And Meterage
关键词
保健食品
七烯甲萘醌
脂肪酶
高效液相色谱
health food
menatetrenone 7(MK-7)
lipase
high performance liquid chromatography
作者简介
通信作者:张彦,教授级高工,博士,研究方向为食品营养与功能。
