陈汉峰
（捷通（广州）检测技术服务有限公司，广东 广州 510730）
摘要：目的：建立超临界色谱法测定营养补充片剂中维生素D2、D3、K1 和K2 含量的分析方法。方法样品经二甲基亚砜（Dimethyl sulfoxide，DMSO）预处理后，经正己烷提取，氮吹仪吹干溶剂后，再准确移入一定体积甲醇乙腈复溶溶剂，振荡充分溶解后合相色谱分析。选用串联两根色谱柱Waters UPCC HSS C18 SB 2.1mm×100mm 1.8μm，流动相A 为CO2 流动相B 为甲醇乙腈（25：75）混合溶液，梯度洗脱。样品进样量为10μL ，流速为1mL/min，柱温为40 ℃，合相管理器反压为1700psi，于265nm 波长处测定样品。结果：维生素K1、维生素K2、维生素D2 和维生素D3 分别在0.298～7.454μg/L（r2=0.99992）、2.308～57.69μg/L（r2=0.99997）、0.657～16.42μg/L（r2=0.99991）和0.399～9.976 μg/L（r2=0.99990）范围内线性关系良好；回收率在90.0% - 108.6%之间；相对标准偏差在1.0%-6.1%之间；维生素K1、维生素K2、维生素D2 和维生素D3 检出限分别为0.007mg/kg、0.011mg/kg、0.011mg/kg、0.011mg/kg，定量限分别为0.021mg/kg、0.033mg/kg、0.033mg/kg、0.033mg/kg。结论该方法快速、稳定，是同时检测营养片剂中维生素D2、D3、K1 和K2 的简单有效的方法。
关键词：超高效合相色谱法；维生素D2；维生素D3；维生素K1；维生素K2；营养补充片剂
Determination of Vitamin D2，D3，K1，and K2 Content in Nutritional Supplement Tabletsby Ultra High Performance Chromatography
CHEN Han-feng
（Access（Guangzhou）Testing Technology Service Co.，Ltd .，Guangzhou 510730，China）
Abstract: Objective：To establish an analytical method for determining the contents of vitamin D2，D3，K1，and K2 innutritional supplement tablets using supercritical chromatography. Method： After pretreatment with Dimethylsulfoxide （DMSO），the sample was extracted with n- hexane，dried with a nitrogen blow dryer，and accuratelytransferred into a certain volume of methanol acetonitrile solvent for reconstitution. After sufficient shaking anddissolution，the mixture was analyzed by phase chromatography. Select two chromatography columns Waters UPCCHSS C18 SB 2.1mm×100mm 1.8μm in series，mobile phase A was CO2，mobile phase B was a mixture of methanoland acetonitrile（25∶75），gradient elution. The sample injection volume was 10μL，the flow rate was 1mL/min，thecolumn temperature was 40℃，and the back pressure of the phase manager was 1700psi. Measure the sample at awavelength of 265 nm. Result：Vitamin K1， vitamin K2， vitamin D2， and vitamin D3 showed good linearrelationships within the ranges of 0.298-7.454μg/mL（r2=0.99992），2.308-57.69μg/mL（r2=0.99997），0.657-16.42μg/mL（r2=0.99991），and 0.399- 9.976μg/mL（r2=0.99990），respectively；The recovery rate was between 90.0% and108.6%；The relative standard deviation was between 1.0% and 6.1%；The detection limits for vitamin K1，vitaminK2，vitamin D2，and vitamin D3 were 0.007mg/kg，0.011mg/kg，0.011mg/kg，and 0.011mg/kg. The quantificationlimits were 0.021mg/kg，0.033mg/kg，0.033mg/kg，and 0.033mg/kg. Conclusion：This method was fast and stable，and was a simple and effective method for simultaneously detecting vitamins D2，D3，K1，and K2 in nutritional tablets.
Key words: ultraperformance convergence chromatography；Vitamin D2；Vitamin D3；Vitamin K1；Vitamin K2；nutritional supplement tablets
中图分类号：TS207 文献标志码：A 文章编号：1007-7871（2024）06-0041-07
2024，Vol.27，No.6