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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.

In this paper an analytical method was developed for the determination of some tobacco specific N-nitrosamines (TSNAs) in cigarettes, and applied to cigarettes purchased in the city of Rio de Janeiro/RJ (Brazil).

Abstract. Currently, due to the strong trends in policies to reduce smoking, several concerns related to quality control and regulation of tobacco products have been raised, as a great variety of products are available to consumers in the market. Considering that development of robust and selective analytical methods for tobacco and derivative products has been an important and necessary task over the years, however laborious, due to the complexity of the matrices. This work presents an overview of advances, innovation, and trends in analytical methods, focused on the chromatographic analysis of nicotine, tobacco-specific nitrosamines (TSNAs), humectants, pesticides, polycyclic aromatic hydrocarbons (PAHs) and sugars in different tobacco products. Gas chromatography (GC) coupled with different detectors is widely used to analyze nicotine, humectants and TSNAs in tobacco leaves and derivative products, while liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been frequently used to analyze TSNAs in mainstream cigarette smoke and smokeless tobacco products. Pesticides were mainly analyzed in tobacco using GC or LC coupled with mass detector (MS), while PAHs and sugars were generally analyzed in tobacco and smoke using LC-MS and GC-MS techniques, respectively. In addition to already established methods and despite the lack of a worldwide standardization of methods, significant efforts have been made to develop analytical procedures for a wide variety of tobacco products, with a broad range of innovative chromatographic methods available. In this sense, a potential trend is the possibility of simultaneous determination of multiple components aiming to reduce the analysis time. The present study examined the main works that developed or improved analytical methods for identifying and quantifying priority compounds in different tobacco matrices and aims to contribute to future research with this objective, in addition, to promoting standardization of technical terms used in this analytical area. It is noteworthy that some of the methods mentioned here have not been validated and further studies are needed in order to obtain reproducible analytical methods for regulatory purposes. Keywords: chromatography analyses; tobacco leaves; cigarette; cigarette smoke; smokeless tobacco products.

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