高效液相色谱法测定微胶囊化片剂型保健食品中VK2的含量

Determination of vitamin K2 in microencapsulated tablet-type health products by high performance liquid chromatography

建立高效液相色谱法测定微胶囊化保健品片剂中VK2(七烯甲萘醌)的分析方法。样品使用添加了稀盐酸溶液进行破壁,破坏维生素片的微胶囊化包裹,使目标物充分游离,再用无水乙醇提取游离态的VK2,采用Thermo scientific Vitade-004K1色谱柱进行分离,以100%甲醇为流动相进行等度洗脱,用二极管阵列检测器在波长254nm处进行检测,外标法定量。结果表明:VK2(七烯甲萘醌)保留时间为4.2min,当取样量为1g时,VK2(七烯甲萘醌)检出限为0.52μg/100g,在0.20-2.0μg/mL范围内线性良好,相关系数R2=0.99991,3个浓度级别的回收率为91.2%-94.1%之间;相对标准偏差(RSD)≤1.11%,该方法准确性高、重现性好、操作简单,可用于微胶囊化片剂型保健食品中VK2的测定。

An analytical method for the determination of vitamin K2(heptene menadione)in microencapsulated health product tablets was established by high performance liquid chromatography.The sample was broken by adding dilute hydrochloric acid solution to destroy the microencapsulation package of the vitamin tablets,so that the target substance was fully freed,and then the free vitamin K2 was extracted with absolute ethanol,and separated by a Thermo scientific vitade-004K1 column.100%Methanol was used as the mobile phase for isocratic elution,detected by a diode array detector at a wavelength of 254 nm,and quantified by an external standard method.The results showed that the retention time of vitamin K2(heptene menadione)was 4.2min.When the sampling amount was 1g,the detection limit of vitamin K2(heptene menadione)was 0.52μg/100g,which was between 0.20-2.0μg/mL The linearity in the range is good,the correlation coefficient R2=0.99991,the recovery rate of the 3 concentration levels was between 91.2%and 94.1%;the relative standard deviation(RSD)≤1.11%,the method had high accuracy,good reproducibility,and simple operation It can be used for the determination of vitamin K2 in microencapsulated tablet health food.