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Desenvolvimento de um método analítico para quantificação de um intermediário de API
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Minocycline hydrochloride is an API synthesized in Cipan over 7 production steps. The 4th step is considered to be the key step of the process, when the 7-HT molecule is formed. It was verified that the variability between 7-HT’s batches is reflected on the quality of the final product becoming fundamental the effective analysis of this intermediate. The existent analytical method for this intermediate is not validated, and it has limitations like the high flow rate of 3mL/min and 70 minutes of analysis, generating high solvents consumption and high pressures in the system, being harmful to the system.
In this project was developed a new analytical method for identification and quantitation of 7-HT and it’s related substances, using a C-8 column instead of the current one which is a C-18, resulting in a lower analyte’s retention. Applying a gradient elution mode and a flow rate of 1 mL/min, it was possible to reduce the analysis time to 40 minutes. This method uses a mobile phase compatible with LC-MS, allowing the identification of unknown peaks. The application of statistical methods, namely as F test to analyze the variances, and the t test for paired data differences allowed the comparison of the results obtained by the two methods. It was also possible to standardize a 7-HT sample through qNMR, with 86,8% of purity, and to make the secondary standardization of the 7-HT currently used as standard in the HPLC analyzes, with 96,9% of purity, from the primary standard. The linearity of 7-HT was evaluated and proved through the correlation coefficient, residue’s analysis and Mandel's test.
Finally, an economic analysis was performed to compare the cost of each analysis in both methods, which in the original method is 0,86€/run and in the new one is 0,12€/run. In order to use the new method in the analytical control it will be necessary to validate it according to the regulatory guidelines.
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HPLC development LC-MS standardization linearity