Siqueira-Moura M P, Primo F L, Peti A P F, Tedesco A C
Programa de Pós-Graduação em Ciências Farmacêuticas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto (FCFRP), Universidade de São Paulo, Ribeirão Preto-SP, Brasil.
Pharmazie. 2010 Jan;65(1):9-14.
UV-VIS-Spectrophotometric and spectrofluorimetric methods have been developed and validated allowing the quantification of chloroaluminum phthalocyanine (CIAIPc) in nanocarriers. In order to validate the methods, the linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and selectivity were examined according to USP 30 and ICH guidelines. Linearities range were found between 0.50-3.00 microg x mL(-1) (Y = 0.3829 X [CIAIPc, microg x mL(-1)] + 0.0126; r = 0.9992) for spectrophotometry, and 0.05-1.00 microg x mL(-1) (Y = 2.24 x 10(6) X [CIAIPc, microg x mL(-1)] + 9.74 x 10(4); r = 0.9978) for spectrofluorimetry. In addition, ANOVA and Lack-of-fit tests demonstrated that the regression equations were statistically significant (p<0.05), and the resulting linear model is fully adequate for both analytical methods. The LOD values were 0.09 and 0.01 microg x mL(-1), while the LOQ were 0.27 and 0.04 microg x mL(-1) for spectrophotometric and spectrofluorimetric methods, respectively. Repeatability and intermediate precision for proposed methods showed relative standard deviation (RSD) between 0.58% to 4.80%. The percent recovery ranged from 98.9% to 102.7% for spectrophotometric analyses and from 94.2% to 101.2% for spectrofluorimetry. No interferences from common excipients were detected and both methods were considered specific. Therefore, the methods are accurate, precise, specific, and reproducible and hence can be applied for quantification of CIAIPc in nanoemulsions (NE) and nanocapsules (NC).
已开发并验证了紫外可见分光光度法和荧光分光光度法,可用于定量纳米载体中的氯铝酞菁(CIAIPc)。为了验证这些方法,根据美国药典30版和国际人用药品注册技术协调会(ICH)指南,对线性、检测限(LOD)、定量限(LOQ)、精密度、准确度和选择性进行了考察。分光光度法的线性范围为0.50 - 3.00μg x mL⁻¹(Y = 0.3829X[CIAIPc,μg x mL⁻¹] + 0.0126;r = 0.9992),荧光分光光度法的线性范围为0.05 - 1.00μg x mL⁻¹(Y = 2.24 x 10⁶X[CIAIPc,μg x mL⁻¹] + 9.74 x 10⁴;r = 0.9978)。此外,方差分析(ANOVA)和失拟检验表明回归方程具有统计学意义(p<0.05),所得线性模型对两种分析方法均完全适用。分光光度法和荧光分光光度法的LOD值分别为0.09和0.01μg x mL⁻¹,而LOQ分别为0.27和0.04μg x mL⁻¹。所提出方法的重复性和中间精密度显示相对标准偏差(RSD)在0.58%至4.80%之间。分光光度分析的回收率为98.9%至102.7%,荧光分光光度法的回收率为94.2%至101.2%。未检测到常见辅料的干扰,两种方法均具有特异性。因此,这些方法准确、精密、特异且可重现,可用于定量纳米乳剂(NE)和纳米胶囊(NC)中的CIAIPc。