Intralaboratory validation, comparison and application of HPLC-UV-DAD methods for simultaneous determination of benzalkonium chloride, chlorexidine digluconate and triclosan
Abstract:Cloreto de benzalcônio (BAC), digluconato de clorexidina (CD) e triclosan (TR) são amplamente usados como agentes antimicrobianos já que são anti-sépticos e desinfetantes, dependendo da concentração. O objetivo deste trabalho foi o desenvolvimento de metodologia para a determinação rápida e simultânea de CD, TR e dos homólogos do BAC (C 12 , C 14 e C 16 ) por CLAE-UV-DAD. Dois sistemas isocráticos em fase reversa foram otimizados: sistema C8 -coluna SB-C8 (250 × 4,6 mm; 5 µm) e fase móvel composta por ACN e ta… Show more
“…Algunas técnicas para la determinación de TCS incluyen la cromatografía de líquidos de alta eficiencia (HPLC) (Sanches- Silva et al, 2005) acoplado a espectrometría de masas (HPLC-MS) (Shen et al, 2012), y cromatografía de gases acoplado a espectrometría de masas (GC-MS) (Wu et al, 2007). Las técnicas mencionadas, HPLC es la herramienta más práctica y sencilla para la determinación de TCS en productos de cuidado personal (Piccoli et al, 2002;Chiapetta et al, 2011;Liu & Wu, 2012). En este artículo, se presenta un método analítico económico, simple y rápido para determinar TCS en muestras de pasta de dientes usando HPLC con detector de arreglo de diodos.…”
Triclosan (TCS) is used in many health care products as a broad-spectrum antimicrobial and disinfectant agent; however, it is currently considered an emerging pollutant. The present study aimed to develop an analytical HPLC method coupled to a Diode Array Detector for the TCS determination in toothpaste. Method development involved the optimization of separation and sample preparation. For chromatographic separation optimization, different RP columns and aqueous mobile phases were addressed. The optimized chromatographic separation was achieved in around 3 minutes using a Symmetry C18 column at 30 °C, 0.6 mL/min flow-rate, and 225 nm wavelength detection. For toothpaste sample preparation optimization a response surface methodology using a Box-Behnken fractional factorial design was chosen. The sample treatment consisted of leaching 0.2 g sample by sonication for 7 minutes using 2 mL of MeOH. According to the International Conference on Harmonization (ICH, 1996/2005) and European Commission Decision 200/657/EC guidelines, the developed method was validated. The developed analytical method was found fast, economic, linear, sensitive, precise, and robust and allowed to quantify TCS in different healthcare products.
“…Algunas técnicas para la determinación de TCS incluyen la cromatografía de líquidos de alta eficiencia (HPLC) (Sanches- Silva et al, 2005) acoplado a espectrometría de masas (HPLC-MS) (Shen et al, 2012), y cromatografía de gases acoplado a espectrometría de masas (GC-MS) (Wu et al, 2007). Las técnicas mencionadas, HPLC es la herramienta más práctica y sencilla para la determinación de TCS en productos de cuidado personal (Piccoli et al, 2002;Chiapetta et al, 2011;Liu & Wu, 2012). En este artículo, se presenta un método analítico económico, simple y rápido para determinar TCS en muestras de pasta de dientes usando HPLC con detector de arreglo de diodos.…”
Triclosan (TCS) is used in many health care products as a broad-spectrum antimicrobial and disinfectant agent; however, it is currently considered an emerging pollutant. The present study aimed to develop an analytical HPLC method coupled to a Diode Array Detector for the TCS determination in toothpaste. Method development involved the optimization of separation and sample preparation. For chromatographic separation optimization, different RP columns and aqueous mobile phases were addressed. The optimized chromatographic separation was achieved in around 3 minutes using a Symmetry C18 column at 30 °C, 0.6 mL/min flow-rate, and 225 nm wavelength detection. For toothpaste sample preparation optimization a response surface methodology using a Box-Behnken fractional factorial design was chosen. The sample treatment consisted of leaching 0.2 g sample by sonication for 7 minutes using 2 mL of MeOH. According to the International Conference on Harmonization (ICH, 1996/2005) and European Commission Decision 200/657/EC guidelines, the developed method was validated. The developed analytical method was found fast, economic, linear, sensitive, precise, and robust and allowed to quantify TCS in different healthcare products.
“…A number of analytical methods have been reported for the estimation of BKC in various products including ophthalmic preparations [7][8][9][10][11][12][13][14][15][16][17][18][19][20][21][22][23]. However, there was no method available for estimation of BKC in azelastine hydrochloride ophthalmic formulations.…”
Objective: This study was designed to conduct forced degradation and validation studies for determination the benzalkonium chloride (BKC) as major homologues form in azelastine hydrochloride pharmaceutical ophthalmic formulation by a novel stability indicating reverse phase high-performance liquid chromatographic method (RP-HPLC).Methods: Forced degradation study and validation were carried out with a analytical approach of reverse phase chromatographic analysis with C18, cosmosil (250mm x 4.6mm i.d. x 5µm) column using mobile phase consisting acetonitrile -buffer of pH 5.0 with 5N NaOH (45:55 %v/v) at a flow rate of 1.5 ml per minute. Column temperature was maintained at 25°C and detection wavelength was 210nm.By using these chromatographic conditions of method, two major homologues of benzalkonium chloride were separated without any interference of drug components and exciepients.Results: Forced degradation studies were carried out as per ICH guidelines and established a stability indicating property of a method .The method was found linear in concentration range 40µg/ml to 60µg/ml (50µg/ml±20%), correlation coefficient was found 0.999. The recovery was found to be 99.2%, 100.7% and 101.4% at ±30% of target concentration. The %RSD for method precision and intermediate precision were found 0.28% and 0.30 % respectively. The method was found specific, selective, precise, accurate, linear, robust and stability indicating for quantification benzalkonium chloride in azelastine pharmaceutical ophthalmic formulation.
Conclusion:The method has been found successful for determination of BKC pharmaceutical formulation and validated for all the parameters of validation and found within the acceptance criteria as per ICH guideline Q2R1.
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