研究目的
The aim of this study is the proposition of LIBS as an analytical technique of tablets composed mainly of dipyrone, due to the presence and distribution homogeneity of its active pharmaceutical ingredients (APIs) and excipients.
研究成果
This study has allowed us to validate the LIBS technique as an analyzing method and it has enabled us to increase employment fields, extending them to investigate pharmaceuticals. In this way, it is possible to observe its versatility in different matrix studies.
研究不足
This technique is subject to problems like matrix effects, sample geometry and instrumentation, which restrict its reproducibility and result in uncertainties in plasma characterization and qualitative analysis of indicated elements.
1:Experimental Design and Method Selection:
A single pulse LIBS setup was used to assess tablet homogeneity. All data were obtained using a nanosecond 1064 nm Nd:YAG Q-switched laser with 50 mJ of laser pulse energy with durations of 8 ns and spot size of 150 μm on the sample surface. The spectral analysis was performed by a CCD spectrometer composed of six detectors with a spectral window of 186 ? 1042 nm (12 288 emission lines with resolution in the range of
2:050 ? 094 nm) with a delay time (between laser pulse and detection) of 1 μs. A xyz translational ablation chamber with a 1280-1024 CMOS color camera imaging system was used to perform the ablation pattern. Sample Selection and Data Sources:
The sample used was a very common medicine found on the Brazilian market, employed for headaches, fever, stressed muscles and pain in general. Its analgesic and antipyretic effects are due to one of its APIs: dipyrone (metamizol, C13H16N30SNa).
3:List of Experimental Equipment and Materials:
Applied Spectra, model J200, USA; Quantel Ultra, USA; Axiom
4:5 software. Experimental Procedures and Operational Workflow:
The chosen region in the target was a 10 × 10 matrix (ablation pattern), where each point received 11 laser pulses. A total of 1100 LIBS spectra in each sample was obtained. The first pulse was used to clean the sample surface and its information was discarded.
5:Data Analysis Methods:
The obtained LIBS spectra were analyzed for each region with a homemade MATLAB routine and the lines of interest (C, Na, Mg and Fe) were identified using the National Institute of Standards and Technology (NIST) database.
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