Full text
| |
| Author(s): |
Maiara da Silva Santos
Total Authors: 1
|
| Document type: | Doctoral Thesis |
| Press: | São Carlos. |
| Institution: | Universidade de São Paulo (USP). Instituto de Química de São Carlos (IQSC/BT) |
| Defense date: | 2014-02-14 |
| Examining board members: |
Luiz Alberto Colnago;
Roberto Gomes de Souza Berlinck;
Daniel Rodrigues Cardoso;
Sonia Maria Cabral de Menezes
|
| Advisor: | Luiz Alberto Colnago |
| Abstract | |
The need for effective and reliable quality control in products and/or raw materials from pharmaceutical and agricultural industries make analyses of their actives compounds and constituents very important to manufacturers and consumers. Nuclear Magnetic Resonance spectroscopy (NMR) is one of the most important tools for qualitative analysis but it is rarely used as quantitative method. Considering these facts, quantitative NMR methods (qNMR) for analysis of pharmaceutical and agricultural products were developed in this thesis. A high resolution 1H qNMR method for paracetamol, in different pharmaceutical formulations, was validated according to RE Resolution Nº 899. An internal standard was used in this method, therefore, the construction of a calibration curve was unnecessary. Other actives constituents present in the formulations could also be quantified and some excipients, identified. According to NBR 14029, high resolution qNMR 1H and 31P methods were developed and validated for glyphosate. In this case, an external standard was used, which enabled sequential quantitative analyses of different nuclei without the need to prepare a new sample. The high-resolution qNMR 1H was also used as an alternative method for fatty acids determination in oils and olive oils, dispensing transesterifications reactions required for GC analysis. Time domain NMR (TD-NMR) was used to develop a method to detect adulteration of olive oil with soybean oil. This method was based on the viscosity difference between olive oil and soybean oil, and has a great advantage, because it can be applied in sealed packages. Finally, different analytical approaches using high resolution NMR 1H were studied to qualitative and quantitative analysis of milk thistle (Silybum marianum L. Gaertn., Asteraceae), a botanical dietary supplement, enabling the simultaneous quantification of seven active constituents, including two pairs of diastereoisomers. Therefore, it was demonstrated in this thesis the potential of qNMR techniques to quality control of pharmaceutical and agricultural products, with some advantages over other analytical methods, normally used in these analyses. (AU) | |
| FAPESP's process: | 11/18032-0 - Development and validation of quantitative NMR methods for drugs, agrochemicals and olive oils analyses |
| Grantee: | Maiara da Silva Santos |
| Support Opportunities: | Scholarships in Brazil - Doctorate |