Новые возможности количественного хроматографического анализа методом двойного внутреннего стандарта

Abstract

One of the methods of chromatographic quantitation of analytes in complex matrices with sorption properties is the modified double standard method. It implies introducing the two homologues of target analytes into original samples. This mode provides the high accuracy of determinations despite of any losses of their constituents at all stages of sample preparation. The application of this method is illustrated on the examples of model samples prepared by adding of polar alkanecarboxylic acids to the polar sorbent Silipor 75 (LaChema, Check Republic) followed by their extraction and conversion into derivatives (ethyl esters) for gas chromatographic determination. Relative errors of this mode are (-1) – (-8) %, that is significantly less than those of other possible methods. It is shown this method is applicable at the presence of homologues of analytes in the initial samples, and it can be generalized onto any number of carbon atoms in the molecules of selected standards. The single principal restriction of the double internal standard method remains to be practical availability of the reference samples of homologues. Key words: Quantitative chromatographic analysis, matrix effects, sample preparation, losses of analytes, desorption, extraction, derivatization, double internal standard method. (Russian) DOI: http://dx.doi.org/10.15826/analitika.2014.18.4.014 Igor G. Zenkevich, Konstantin M. Korolev St. Petersburg State University, St. Petersburg, Russian Federation REFERENCES 1. Novak J. Quantitative Analysis by Gas Chromatography . New York: Marcel Dekker Inc., 1975. 130 p. 2. Stolyarov B.V., Savinov I.M., Vitenberg A.G., Kartsova L.A., Zenkevich I.G., Kalmanovskii V.I., Kalambet Yu.A. Prakticheskaia gazovaia i zhidkostnaia khromatografiia [Practical Gas and Liquid Chromatography]. St. Petersburg, Univ. Press, 2002. 610 p. (in Russian). 3. Grob R.L., Barry E.F. Modern Practice of Gas Chromatography . 4 th Edn. 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