胶束液相色谱法测定药品和预混剂中的硒（IV）

Determination of selenium(IV) in pharmaceuticals and premixes by micellar liquid chromatography.

作者信息

Kulikov Artem U

机构信息

Laboratory of Pharmacopoeial Analysis, Scientific and Expert Pharmacopoeial Centre, Astronomicheskaya street 33, 61085 Kharkov, Ukraine.

出版信息

J Pharm Biomed Anal. 2007 Mar 12;43(4):1283-9. doi: 10.1016/j.jpba.2006.10.041. Epub 2006 Dec 5.

DOI:10.1016/j.jpba.2006.10.041

PMID:17156959

Abstract

A simple micellar liquid chromatographic technique for the determination of selenium(IV) in pharmaceutical products (multi-vitamin tablets, syrups) and animal premixes after pre-column derivatization with 2,3-diaminonaphthalene was developed and validated. Hypersil ODS column, 10% (v/v) 1-butanol in 0.05 M sodium dodecyl sulfate as the mobile phase and UV detection at 378 nm and were used. The retention time was about 8 min. In the course of the validation study, the specificity of the method was demonstrated. Linearity was established in the range 0.33-3.3 microg ml(-1) of selenium(IV) content. The limits of detection and quantitation were 0.1 and 0.3 microg ml(-1), respectively. The method showed excellent accuracy (100.04%). Precision (repeatability) gave a relative standard deviation less than 1%. The influence of the various method parameters (robustness study) was also investigated.

摘要

建立并验证了一种简单的胶束液相色谱技术，用于在2,3-二氨基萘柱前衍生化后测定药品（多种维生素片、糖浆）和动物预混料中的硒（IV）。使用Hypersil ODS柱，以0.05 M十二烷基硫酸钠中10%（v/v）的1-丁醇为流动相，并在378 nm处进行紫外检测。保留时间约为8分钟。在验证研究过程中，证明了该方法的特异性。在硒（IV）含量为0.33 - 3.3 μg ml⁻¹的范围内建立了线性关系。检测限和定量限分别为0.1和0.3 μg ml⁻¹。该方法显示出优异的准确度（100.04%）。精密度（重复性）的相对标准偏差小于1%。还研究了各种方法参数的影响（稳健性研究）。