ABSTRACT
An analytical method based on capillary electrophoresis (CE) with a partially aqueous electrolyte system was developed to enable the free fatty acids of Brazil nut oil to be identified in cosmetic formulations. In this study, a gel cream formulation was developed and its oil phase was extracted with a mixture of chloroform-methanol-water (1:2:0.8 v/v/v). The chloroform layer was saponified with a methanolic solution of NaOH (0.5 mol L-1) at 75-80 °C for 25 minutes. Experiments were carried out on a Beckman PACE/MDQ CE system (Fullerton, CA, USA) equipped with an on-column, diode-array detection system set at 254 nm and at 25ºC. The electrolyte consisted of 12.5 mmol L-1 sodium tetraborate buffer pH 7.0, 12.5 mmol L-1 polyoxyethylene 23-lauryl ether, 7.5 mmol L-1 sodium dodecylbenzenesulfonate (used as chromophore for indirect UV detection) and acetonitrile (35% v/v). The proposed method allowed the separation and identification of the fatty acids of Brazil nut oil in a cosmetic gel cream, as well as enabling possible interference by the oily phase components in the formulation to be identified.
Um método de análise por eletroforese capilar com sistema de eletrólito parcialmente aquoso foi desenvolvido para identificar os ácidos graxos livres do óleo de Castanha do Brasil em formulações cosméticas. No presente trabalho foi desenvolvida uma formulação cosmética (gel creme) cuja fase oleosa foi extraída com uma mistura de clorofórmio-metanol-água (1:2:0.8 v/v/v). A camada de clorofórmio, foi saponificada com solução de NaOH em metanol (0,5 mol L-1) a 75-80 °C durante 25 minutos. Os experimentos foram realizados em sistema de eletroforese capilar Beckman PACE/MDQ (Fullerton, CA, USA), com detecção de arranjo de diodos a 254 nm e a 25 ºC. O eletrólito utilizado foi 12,5 mmol L-1 de tetraborato de sódio tampão a pH 7,0, 12,5 mmol L-1 de éter de polioxietileno 23-lauril, 7,5 mmol L-1 de dodecilbenzenosulfonato de sódio (utilizado como agente cromóforo para detecção UV indireta) e acetonitrila (35% v/v). O método proposto permitiu a separação e a identificação dos ácidos graxos do óleo de Castanha do Brasil em formulações cosméticas, bem como possibilitou a identificação de interferências presentes na fase oleosa da formulação.
Subject(s)
Cosmetics , Electrophoresis, Capillary , Fatty AcidsABSTRACT
A high performance liquid chromatographic (HPLC) and a ultraviolet derivative spectrophotometric (UVDS) methods were developed and validated for the quantitative determination of hydroquinone (HQ) in gels and creams containing this compound as a unique active principle. Validation parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD) and limit of quantitation (LOQ) were determined. HPLC was carried out by reversed phase technique on a RP-18 column with a mobile phase composed of methanol and water (20:80, v/v). The linearity in the range of 6.0-30.0 microg/mL present a correlation coefficient (r) of 0.9999, calculated by least square method. The LOD and LOQ were 0.08 and 0.26 microg/mL, respectively. Based on the preliminary spectrophotometric profile of HQ, a signal at 302.0 nm of the first derivative spectrum (1D302.0) was found adequate for validation. The linearity between signal 1D302.0 and concentration of HQ in the range of 10.0-26.0 microg/mL in sulfuric acid (0.1N) present a correlation coefficient (r) of 0.9999. The LOD and LOQ were 0.14 and 0.46 microg/mL, respectively. Statistical analysis by t- and F-tests, showed no significant difference at 95% confidence level between the two proposed methods.