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作 者:李丹凤 黄罗健 朱健萍 卢日刚 LI Dan-feng;HUANG Luo-jian;ZHU Jian-ping;LU Ri-gang(Guangxi Institute for Food and Drug Control,Nanning 530021,China;College of Pharmacy,Guilin Medical University,Guilin 541100,China)
机构地区:[1]广西壮族自治区食品药品检验所,广西南宁530021 [2]桂林医学院药学院,广西桂林541100
出 处:《分析测试学报》2020年第9期1155-1159,共5页Journal of Instrumental Analysis
基 金:广西重点研发计划资助项目(桂科AB18221125);2018年广西壮族自治区食品药品安全科研项目资助(桂食药科2018-4直属)。
摘 要:建立了胶束电动色谱(MEKC)法通过波长切换同时测定五维他口服溶液中的维生素B1、B2、B6、烟酰胺、泛酸钙及苯甲酸钠含量的方法,并优化了检测波长、十二烷基硫酸钠(SDS)的浓度、分离电压、缓冲液浓度及pH值等实验条件。最佳分离条件为以未涂渍的标准熔融石英毛细管柱(75μm×50 cm,有效长度42 cm)为分离通道;40 mmol/L硼酸+40 mmol/L硼砂+20 mmol/L SDS(pH 9.0)为运行缓冲液,分离电压20 kV,柱温25℃,检测波长为270 nm(维生素B1、B2、B6、烟酰胺及苯甲酸钠)和200 nm(泛酸钙),电动进样10 kV、进样时间10 s。结果显示,6种化合物可在13 min内实现基线分离,且在一定质量浓度范围内线性良好,相关系数(r)不小于0.9989;3个加标水平下的平均回收率为97.0%~103%,RSD为0.60%~1.8%。该方法快速、准确,可用于五维他口服溶液中维生素B1、B2、B6、烟酰胺、泛酸钙及苯甲酸钠的含量测定。A micellar electrokinetic chromatography(MEKC)with multiwavelength switching was established for the simultaneous determination of vitamin B1,B2,B6,nicotinamide,calcium pantothenate and sodium benzoate in Five Vitamins Oral Solution.Factors affecting separation efficiency such as detection wavelength,concentration of sodium dodecyl sulfate(SDS),separation voltage of sample,pH value and concentration of background buffer were optimized.An optimal separation of six compounds was obtained on an uncoated fused silica capillary column(75μm×50 cm,effective length 42 cm),with a background buffer composed of 40 mmol/L borax+40 mmol/L boric acid+20 mmol/L SDS(pH 9.0),at a separation voltage of 20 kV and a column temperature of 25℃.The detection wavelength was set at 270 nm for vitamin B1,B2,B6,nicotinamide and sodium benzoate,and 200 nm for calcium pantothenate.The sample was electrokinetically injected at 10 kV for 10 s.Results indicated that the six analytes could be separated within 13 min,while their calibration curves showed good linear relationships in the respective concentration ranges,with correlation coefficients(r)not less than 0.9989.The average recoveries at three spiked levels ranged from 97.0%to 103%,with relative standard deviations(RSD)of 0.60%-1.8%.The method is rapid,accurate and reliable,and could be used for the determination of vitamin B1,B2,B6,nicotinamide,calcium pantothenate and sodium benzoate in Five Vitamins Oral Solution.
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