Banca de QUALIFICAÇÃO: ANA ROBERTA PEREIRA JOHNSON DOS ANJOS

Uma banca de QUALIFICAÇÃO de MESTRADO foi cadastrada pelo programa.
STUDENT : ANA ROBERTA PEREIRA JOHNSON DOS ANJOS
DATE: 30/09/2025
TIME: 14:00
LOCAL: VIDEOCONFERÊNCIA
TITLE:

Simultaneous analysis of synthetic peptides stigmurin, StigA8, TsAP-2, and

TistH by high- and ultra-high-performance chromatographic separation techniques coupled to high-resolution mass analyzers

KEY WORDS:

analytical quality by design; method development; peptides; Tityus stigmurus; UHPLC-MS-ESI-TOF.

PAGES: 151
BIG AREA: Ciências da Saúde
AREA: Farmácia
SUMMARY:

This study aimed to develop a robust chromatographic method for the simultaneous

analysis of Tityus stigmurus scorpion peptides, investigating the influence of

operational factors on the method's quality and effectiveness. To achieve this purpose,

a Quality by Design (QbD) methodology was applied, using Design of Experiments

(DoE) for a multifactorial plan that included a screening phase followed by an

optimization phase. Analyses were performed on a UHPLC/MS-ESI TOF system, and

the data were processed with Statistica and Design-Expert software, employing

analysis of variance (ANOVA) and response surface plots to delineate the Method

Operable Design Region (MODR). The results confirm that the selection of a core-shell

particle technology column provided a higher number of theoretical plates (N) and

better peak symmetry, resulting in resolutions greater than 2 for all critical pairs. The

optimization plan analysis demonstrated that the proportion of the organic mobile

phase (%B) is the most impactful factor on resolution and retention time, with the 40-

42% B range being ideal for maximizing the design space. The statistical models

developed were validated by parameters such as a significant p-value, high R²

coefficients, and adequate precision. Multiple ideal separation conditions were

identified, with analysis times ranging from 6 to 20 minutes. In conclusion, the study

demonstrates the successful application of QbD for the development of a flexible and

high-performance analytical method, proving its effectiveness in optimizing

chromatographic processes for peptide separation.

COMMITTEE MEMBERS:
Externo ao Programa - 2140814 - FERNANDO HENRIQUE ANDRADE NOGUEIRA - nullExterna à Instituição - LILIAN GRACE DA SILVA SOLON - UNIFAP
Presidente - 1544647 - MATHEUS DE FREITAS FERNANDES PEDROSA