摘要
建立了一种新的微乳体系,并成功地应用于微乳液相色谱法(MELC)快速分析脂溶性维生素VA、VD2、VD3和VE。通过对影响分离选择性的主要因素进行考察,得到最佳微乳体系组成为98%(v/v)(50 g/L十二烷基硫酸钠(SDS)-10%(质量分数)正丁醇-1.0%(质量分数)正辛烷-84%水(质量分数))-2%(v/v)乙腈。该微乳体系中,表面活性剂类型和浓度、油相正辛烷的含量、有机添加剂乙腈对脂溶性维生素的分离起到了重要的作用。以VenusilASB C18色谱柱(150 mm×4.6 mm,5μm)为分离柱,流速为0.7 mL/min,检测波长为265 nm,柱温为40℃,VA、VD2、VD3和VE在20 min内达到基线分离。4种脂溶性维生素的保留时间和峰面积的相对标准偏差(RSD)(n=5)分别小于2.3%和3.0%;VA、VD2、VD3和VE的线性范围分别为22.0～88.0 mg/L、20.2～81.0 mg/L、24.3～97.2mg/L和125.0～500.0 mg/L,相应的线性相关系数r2分别为0.999 6、0.999 4、0.999 8、0.999 8;检出限(S/N=3)分别为0.37、0.34、0.41和2.12 mg/L。本方法已成功应用于多维元素片(21)中VA与VE的测定,结果令人满意。
A novel system was developed for the rapid determination of fat-soluble vitamins A,D2,D3 and E with microemulsion liquid chromatography（MELC）.The effects of operating parameters on the separation selectivity were investigated.The optimized microemulsion system consisted of 98%（v/v） of 50 g/L sodium dodecyl sulfate（SDS）-10%（w/w） n-butanol-1.0%（w/w） n-octane-84% water（w/w） and 2%（v/v） acetonitrile.The type and content of surfactant,the content of oil phase and the organic additive（acetonitrile） were found to play important roles in the separation of four fat-soluble vitamins.The four analytes were baseline separated within 20 min on a Venusil ASB C18 column（150 mm×4.6 mm,5 μm） with a flow rate of 0.7 mL/min and the detection wavelength of 265 nm at 40 ℃.The relative standard derivations（RSDs,n=5） of retention times and peak areas of the analytes were less than 2.3% and 3.0%,respectively.The linear ranges of vitamins A,D2,D3 and E were 22.0-88.0 mg/L,20.2-81.0 mg/L,24.3-97.2 mg/L and 125.0-500.0 mg/L,with their correlation coefficients（r2） of 0.999 6,0.999 4,0.999 8 and 0.999 8,respectively.The detection limits（S/N=3） were 0.37,0.34,0.41 and 2.12 mg/L,respectively.This method was successfully applied to the determination of commercial Vitamins with Minerals Tablets（21）,and the results were satisfactory.
出处
《色谱》
CAS
CSCD
北大核心
2011年第10期995-999,共5页
Chinese Journal of Chromatography
基金
国家自然科学基金项目(81173525)
关键词
微乳液相色谱
微乳流动相
脂溶性维生素
microemulsion liquid chromatography（MELC）
microemulsion mobile phase
fat-soluble vitamins
