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

被引:44
作者
Arantes de Carvalho, Gabriel Gustinelli [2 ]
Nunes, Lidiane Cristina [2 ,3 ]
de Souza, Paulino Florencio [2 ]
Krug, Francisco Jose [2 ]
Alegre, Thaisa Correia [1 ]
Santos, Dario, Jr. [1 ]
机构
[1] Univ Fed Sao Paulo, BR-09972270 Diadema, SP, Brazil
[2] Univ Sao Paulo, Ctr Energia Nucl Agr, BR-13416000 Piracicaba, SP, Brazil
[3] Univ Fed Sao Carlos, Dept Quim, BR-13565905 Sao Carlos, SP, Brazil
关键词
QUANTITATIVE-ANALYSIS; MULTIELEMENT ANALYSIS; MAGNESIUM STEARATE; FLAME AAS; SPECTROSCOPY; NANOSECOND; UNIFORMITY; ELEMENT; PB; CD;
D O I
10.1039/c000703j
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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.
引用
收藏
页码:803 / 809
页数:7
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