Chromatographic quantitation at losses of analyte during sample preparation. Application of the modified method of double internal standard.
Known methods of quantitative chromatographic analysis (calibration, external standard, internal standard and standard addition) require the application of sample preparation techniques without significant losses of analytes. If this condition cannot be satisfied, the compensation of these losses should be provided. The modification of known method of quantitative chromatographic analysis (double internal standard), implying the addition of two homologues (previous and following) of target analytes as internal standards into initial samples is considered. This approach permits us to compensate significant losses both analytes and standards at all stages of sample preparation. The advantages of this method are demonstrated on the examples of liquid-liquid extraction, head space analysis (HSA), distillation of volatile compounds with volatile solvents (concentration in condensates) and evaporation of volatile solvents (concentrating in the residues of solvents). In all cases the application of two homologues as internal standards provides accurate results (the typical relative errors are within 1-6%) at the values of a factor of composition distortion of initial samples (K', the definition is suggested) from 0.2 up to 4. These results are in accordance with general relationships between variations in any physicochemical properties of organic compounds within homologous series. The single found exception was the evaporation of volatile solvents (the open phase transition process) when to get the results with relative errors not more then +10% requires the minimal changes in the composition of initial samples (K' values should not be more then approximately 1.5).
Zenkevich
Igor G
IG
St. Petersburg State University, Chemical Research Institute, Universitetsky pr. 26, St. Petersburg 198504, Russia. izenkevich@mail15.com
Makarov
Evgeny D
ED
D002138:Calibration; D002845:Chromatography / Q000379:methods* / Q000592:standards*; D007700:Kinetics; D008956:Models, Chemical; D012015:Reference Standards; D015203:Reproducibility of Results