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[微乳液液相色谱法同时测定四种脂溶性维生素]

[Simultaneous determination of four fat-soluble vitamins by microemulsion liquid chromatography].

作者信息

Yang Jianrui, Huang Lina, Huang Guangliang, Li Ning

机构信息

Guangdong College of Pharmacy, Guangzhou 510006, China.

出版信息

Se Pu. 2011 Oct;29(10):995-9.

Abstract

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 x4.6 mm, 5 microm) with a flow rate of 0. 7 mL/min and the detection wavelength of 265 nm at 40 degrees C. 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.

摘要

开发了一种用于快速测定脂溶性维生素A、D2、D3和E的新型微乳液液相色谱(MELC)系统。研究了操作参数对分离选择性的影响。优化后的微乳液体系由98%(v/v)的50 g/L十二烷基硫酸钠(SDS)-10%(w/w)正丁醇-1.0%(w/w)正辛烷-84%水(w/w)和2%(v/v)乙腈组成。发现表面活性剂的类型和含量、油相含量和有机添加剂(乙腈)在四种脂溶性维生素的分离中起重要作用。在Venusil ASB C18柱(150 mm×4.6 mm,5μm)上,于40℃、流速0.7 mL/min、检测波长265 nm条件下,20分钟内四种分析物实现了基线分离。分析物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%。维生素A、D2、D3和E的线性范围分别为22.0 - 88.0 mg/L、20.2 - 81.0 mg/L、24.3 - 97.2 mg/L和125.0 - 500.0 mg/L,其相关系数(r2)分别为0.999 6、0.999 4、0.999 8和0.999 8。检测限(S/N = 3)分别为0.37、0.34、0.41和2.12 mg/L。该方法成功应用于复方维生素矿物质片(21)的测定,结果令人满意。

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