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 tampão de H 3 PO 4 /NaH 2 PO 4 0,03 mol L . O tempo de análise foi menor que 6 min em ambos os sistemas, permitindo alta produtividade e baixo uso de solventes. Faixas lineares com duas ordens de magnitude foram obtidas nos dois sistemas. A sensibilidade obtida no sistema C8, para as cinco substâncias foi cerca de 20% maior que no sistema CN. Ambos os métodos apresentaram precisões melhores que 4,5%, boas resoluções (R > 1,8) e altas recuperações (96 a 103%). Os limites de quantificação foram adequados para a determinação das cinco substâncias em produtos comerciais. A análise de diversos produtos comerciais indicou boa concordância entre os métodos cromatográficos e entre ele e os valores rotulados.Benzalkonium chloride (BAC), chlorhexidine digluconate (CD) and triclosan (TR) are widely used antimicrobial agents since they are antiseptics and disinfectants depending on the used concentration. The objective of this work was the development of methodology for the fast and simultaneous determination of CD, TR and the BAC homologues (C 12 , C 14 and C 16 ) using HPLC-UV-DAD. Two isocratic reverse-phase systems were optimized: system C8 -column SB-C8 (250 × 4.6 mm; 5 µm) using a mobile phase composed of ACN and H 3 PO 4 /NaH 2 PO 4 buffer 0.03 mol L . In both systems the total analysis time was lower than 6 min, leading to high throughput and low production of solvent rejects. Linear ranges with two magnitude orders were found for the five substances in both systems. The sensitivity of system C8 for the five substances was around 20% greater than that of system CN. Both chromatographic methods showed overall precisions better than 4.5%, good resolutions (R > 1.8) and high recoveries (96 to 103%). The limits of quantification were adequate for the determination of the five compounds in commercial products. The analysis of several commercial products showed a good agreement between both chromatographic methods. Good agreement among measured concentrations and labeled values was also observed.

EN PRENSA. High Performance Liquid Chromatography coupled Diode Array Detector (HPLC-DAD) method development and validation for the quantification of triclosan in toothpaste. EN PRENSA

“…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.…”

A Study on Forced Degradation and Validation of Stability Indicating Rp-HPLC Method for Determination of Benzalkonium Chloride in Azelastine Hydrochoride Pharmaceutical Ophthalmic Formulation

“…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.…”