Evaluation of dilute-and-shoot procedure for determination of inorganic impurities in liquid pharmaceutical samples by ICP OES

Autor: Ariane I. Barros, Joaquim A. Nóbrega, Fernanda C. Pinheiro
Rok vydání: 2019
Předmět:
Zdroj: Microchemical Journal. 146:948-956
ISSN: 0026-265X
Popis: This study evaluated a dilute-and-shoot procedure for determination of 23 elemental impurities in liquid pharmaceutical samples by inductively coupled plasma optical emission spectrometry (ICP OES). Two dilution factors were tested for analysis of four liquid drugs (10-fold and 20-fold dilution in 0.14 mol L−1 HNO3). Microwave-assisted digestion using 7.0 and 2.0 mol L−1 HNO3 was used for comparison purposes. The accuracy and precision were evaluated by addition-recovery experiments and satisfactory recoveries were obtained only when matrix effects were corrected for applying internal standardization (IS) or one-point standard addition (OP SA) calibration methods. Bismuth, Ge and Y were evaluated as internal standards and recoveries ranged from 86 to 116% when the best internal standard was employed for each analyte. For OP SA, recoveries varied from 78 to 119%. The relative standard deviations for all elements and samples were lower than 9% for both calibration methods applied. The LODs obtained for IS and OP SA were lower than the lower level of addition suggested by the Chapter 233, except for Pb and Tl, and all samples are within the limits recommended by USP considering the maximum daily dose of each liquid drug and the diluted factor adopted in the analytical procedure. The tailored calibration methods were essential to correct for matrix effects enabling application of dilute-and-shoot procedure for samples 10-fold diluted and making feasible the elemental impurities analysis of liquid drugs by ICP OES.
Databáze: OpenAIRE
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