O objetivo deste estudo foi desenvolver e validar um método espectrofotométrico para determinação do LPSF/AC04 em complexo de inclusão e encapsulado em lipossomas. Os parâmetros de validação foram determinados de acordo com o International Conference on Harmonisation (ICH) e Agência Nacional de Vigilância Sanitária (ANVISA). OLPSF/AC04 foi determinado a 250 nm em metanol pelo método espectrofotométrico UV, que apresenta linearidade na faixa de 0,3 a 2 µg/mL (Absorbância = 0,18068 x [LPSF/AC04 µg/mL] + 0,00348), (r2 = 0,9995). Os limites de detecção e quantificação foi 0,047 µg/mL e 0,143 µg/mL, respectivamente. O método foi exato, preciso, reprodutível e robusto e todas as amostras analisadas apresentaram coeficiente de variação menor que 5% e não houve diferença estatisticamente significante entre a concentração teórica e a prática. Assim, um método espectrofotométrico rápido, simples, sensível e de baixo custo foi desenvolvido e validado para determinar o conteúdo do LPSF/AC04 em complexos de inclusão e encapsulados em lipossomas.

The aim of this study was to develop and validate a UV spectrophotometric method for determination of LPSF/AC04 from inclusion complex and encapsulated into liposomes. The validation parameters were determined according to the International Conference on Harmonisation (ICH) and National Health Surveillance Agency (ANVISA) guidelines. LPSF/AC04 was determined at 250 nm in methanol by a UV spectrophotometric method, exhibiting linearity in the range from 0.3 to 2 µg.mL−1 (Absorbance=0.18068 x [LPSF/AC04 µg.mL-1] + 0.00348), (r2=0.9995). The limits of detection and quantification were 0.047µg.mL−1 and 0.143µg.mL−1, respectively. The method was accurate, precise, reproducible and robust since all the samples analyzed had coefficient of variation of less than 5% and no statistically significant difference between theoretical and practical concentrations was detected. Thus, a rapid, simple, low cost and sensitive spectrophotometric method was developed and validated for determining the content of inclusion complex and liposomes containing LPSF/AC04.

This article describes the synthesis of the new (2Z)-2-(4-methoxybenzylidene)-6-nitro-4H -benzo[1,4]thiazin-3-one, (2Z)-2-(4-methoxybenzylidene)-4-methyl-6-nitro-4H-benzo[1,4]thiazin-3-one, (2Z)-6-amino-2-(4-methoxybenzylidene)-4H -benzo[1,4]thiazin-3-one, (2Z)-6-butylamino-2-(4-methoxybenzylidene)-4-methyl-4H-benzo[1,4]-thiazin-3-one and (2E)-N-alkyl-N-(2-hydroxy-5-nitrophenyl)-3-phenylacrylamides and the spectroscopic data. The arylidenebenzothiazine compounds were prepared using the Knoevenagel condensation with substituted benzaldehydes in the presence of sodium methoxide in DMF. The presence of a nitro substituent in the 4-position, water and a slightly acid reaction medium in this condensation caused the rupture of the benzothiazine ring and subsequent formation of the phenylacrylamide compounds. A crystallographic data was presented for (2E)-3-(4-bromophenyl)-N-dodecyl-N -(2-hydroxy-5-nitrophenyl) acrylamide.