Determination of Vitamin D2,D3,K1,and K2 Content in Nutritional Supplement Tablets by Ultra High Performance Chromatography
Objective:To establish an analytical method for determining the contents of vitamin D2,D3,K1,and K2 in nutritional supplement tablets using supercritical chromatography.Method:After pretreatment with Dimethyl sulfoxide(DMSO),the sample was extracted with n-hexane,dried with a nitrogen blow dryer,and accurately transferred into a certain volume of methanol acetonitrile solvent for reconstitution.After sufficient shaking and dissolution,the mixture was analyzed by phase chromatography.Select two chromatography columns Waters UPCC HSS C18 SB 2.1mm×100mm 1.8μm in series,mobile phase A was CO2,mobile phase B was a mixture of methanol and acetonitrile(25∶75),gradient elution.The sample injection volume was 10μL,the flow rate was 1mL/min,the column temperature was 40℃,and the back pressure of the phase manager was 1700psi.Measure the sample at a wavelength of 265 nm.Result:Vitamin K1,vitamin K2,vitamin D2,and vitamin D3 showed good linear relationships 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%and 108.6%;The relative standard deviation was between 1.0%and 6.1%;The detection limits for vitamin K1,vitamin K2,vitamin D2,and vitamin D3 were 0.007mg/kg,0.011mg/kg,0.011mg/kg,and 0.011mg/kg.The quantification limits 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.
NETL
NSTL
万方数据
