Evaluation of laser induced breakdown spectrometry for the determination of macro and micronutrients in pharmaceutical tablets


Autoria(s): CARVALHO, Gabriel Gustinelli Arantes de; NUNES, Lidiane Cristina; SOUZA, Paulino Florencio de; KRUG, Francisco Jose; ALEGRE, Thaisa Correia; SANTOS JR., Dario
Contribuinte(s)

UNIVERSIDADE DE SÃO PAULO

Data(s)

18/10/2012

18/10/2012

2010

Resumo

The aim of this work is to demonstrate the feasibility of laser induced breakdown spectrometry (LIBS) for the determination of macro and micronutrients in multielement tablets. The experimental setup was designed by using a laser Q-switch (Nd:YAG, 10 Hz, lambda = 1064 nm) and the emission signals were collected by lenses into an optical fiber coupled to an echelle spectrometer equipped with a high-resolution intensified charge coupled device (ICCD). Tablets were cryogenically ground and thereafter pelletized before LIBS analysis. Calibration curves were made by employing samples and mixtures of commercial multielement tablets with binders at different ratios. Best results were achieved by using the following experimental conditions: 29 J cm(-2) laser fluence, 165 mm lens to sample distance (f = 200 mm), 2.0 mu s delay time, 5.0 mu s integration time and 5 accumulated laser pulses. In general, the results obtained by the proposed LIBS procedure were in agreement with those obtained by ICP OES from the corresponding acid digests and coefficients variation of LIBS measurements varied from 2 to 16%. The metrological figures of merit indicate that LIBS fits for the intended purposes, and can be recommended for the analysis of multielement tablets and similar matrices aiming the determination of Ca, Cu, Fe, Mg, Mn, P and Zn.

Identificador

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, v.25, n.6, p.803-809, 2010

0267-9477

http://producao.usp.br/handle/BDPI/17014

10.1039/c000703j

http://dx.doi.org/10.1039/c000703j

Idioma(s)

eng

Publicador

ROYAL SOC CHEMISTRY

Relação

Journal of Analytical Atomic Spectrometry

Direitos

closedAccess

Copyright ROYAL SOC CHEMISTRY

Palavras-Chave #QUANTITATIVE-ANALYSIS #EMISSION-SPECTROMETRY #MULTIELEMENT ANALYSIS #SAMPLE INTRODUCTION #MAGNESIUM STEARATE #PLANT MATERIALS #DOSAGE FORMS #FLAME AAS #SPECTROSCOPY #NANOSECOND #Chemistry, Analytical #Spectroscopy
Tipo

article

original article

publishedVersion