高效液相色谱法测定NUSPOWER钙维生素D维生素K口服液中维生素K2含量

Determination of the content of vitamin K2 in NUSPOWER calcium-vitamin D-vitamin K oral liquid by high performance liquid chromatography

中文关键词:  高效液相色谱法  荧光检测器  口服液混悬剂  维生素K2

英文关键词:high performance liquid chromatography  fluorescence detector  oral liquid suspension  vitamin K2

中文摘要:

      目的 建立高效液相色谱法结合荧光检测器测定NUSPOWER钙维生素D维生素K口服液中维生素K2含量的方法。方法 样品经0.1 mol/L盐酸溶液60 ℃水浴超声溶解, 用异丙醇超声提取后, 用混合溶液(500 mL甲醇+100 mL四氢呋喃+0.3 mL冰乙酸+1.5 g氯化锌+0.5 g无水乙酸钠混合超声定容至1000 mL)为流动相, 样品经XSelect?HSS T3 (4.6 mm×250 mm, 5 μm)色谱柱分离, 柱后经锌粉柱(4.6 mm×50 mm)还原, 流速为1.0 mL/min, 进入荧光检测器进行检测。结果 维生素K2即VK2 (MK-7)质量浓度在0.03~0.17 μg/mL范围内呈现良好的线性关系, r2=0.9995, 3个浓度级别的加标回收率在98.40%~102.93%之间, 相对标准偏差为1.6%。结论 该方法前处理简单、准确率高, 可成为口服液混悬剂中维生素K2含量的测定方法。

英文摘要:

      Objective To establish a method for the determination of vitamin K2 content in NUSPOWER calcium-vitamin D-vitamin K oral solution by high performance liquid chromatography combined with fluorescence detector. Methods The sample was dissolved in a 0.1 mol/L hydrochloric acid solution in a 60 ℃ water bath by ultrasound, extracted with isopropanol by ultrasound, and mixed with a mixed solution (500 mL methanol+100 mL tetrahydrofuran+0.3 mL glacial acetic acid+1.5 g zinc chloride+0.5 g anhydrous sodium acetate mixed by ultrasound to a volume of 1000 mL) as the mobile phase. The sample was subjected to XSelect?HSS T3 (4.6 mm×250 mm, 5 μm) chromatographic column separation, followed by reduction on a zinc powder column (4.6 mm×50 mm) at a flow rate of 1.0 mL/min, and detected by a fluorescence detector. Results The mass concentration of vitamin K2, also known as VK2 (MK-7), showed a good linear relationship within the range of 0.03–0.17 μg/mL, with r2=0.9995. The recovery rates of 3 concentration levels were between 98.40%–102.93%, and the relative standard deviations were 1.6%. Conclusion This method is simple and has high accuracy. It can be a method for determining the content of vitamin K2 in oral liquid suspensions.