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Ann. Tabac, Sect. 1-22, 1993, p. 1-10., ISSN.0399-0354

Characterization of mainstream cigarette smoke by HPLC and multivariate statistical analysis of data

SAINT-JALM Y.; NISSERON S.; FAVIER C.
SEITA, Centre de Recherche, Fleury les Aubrais, France
Six HPLC methods for the analysis of tobacco smoke are described in this study. These methods allow then determination of 22 main components of cigarette smoke: The volatile carbonyl compounds are analysed after reaction with 2,4 DNPH (2,4 dinitrophenylhydrazine). The analysis is performed by reversed phase HPLC using a C18 column with a gradient of solvents. Six compounds are determined with this method: formaldehyde, acetaldehyde (ethanal, propionaldehyde (propanal, acrolein (propenal), acetone and butanone; The alpha dicarbonyl compounds are analysed after conversion to the corresponding quinoxalines using ortho-phenylenediamine as reagent. The derivatives are separated in normal phase HPLC on a silica column in isocratic mode. Four compounds are determined with this method: glyoxal, methylglyoxal, diacetyl and 2,3 pentanedione; The aliphatic acids are converted to the corresponding esters with para-bromophenacyl bromide as reagent. The derivatives are separated in reversed phase HPLC with a gradient of solvents. Three acids are determined with this method : formic acid, acetic acid and lactic acid (glycolic acid may be determined with the other acids, but it was not considered in this study); The monophenols are derivatized with 4 aminoantipyrine (4 amino 1,5 dimethyl 2 phenyl 3 pyrazolone). The derivatives are separated in normal phase HPLC on a silica column with isocratic elution. Four compounds are determined with this method: phenol, o + m cresols, gaïacol and 3-hydroxypyridine; The diphenols are derivatised with n butylamine and analysed in normal phase HPLC on a silica column with isocratic elution. Hydroquinone and catechol are determined with this method; The aliphatic amines are derivatised with NBD-Cl (4 chloro 7 nitrobenzo, 2 oxa 1,3 diazole) and analysed on a silica column with isocratic elution. Methyl amine, dimethyl amine and pyrrolidine are determined with this method. In all cases, direct UV detection is used. Thirty-seven commercial cigarette brands were sampled in the European Union (EU) and Switzerland in 1992 and their smoke was analysed with the 6 HPLC methods. The obtained results were then analysed by a combination of different data analysis methods (Principal component analysis, hierarchical clustering and discriminent analysis). The studied samples can be classified into 6 groups of cigarettes and it was demonstrated that 7 determinations are su.fficient to realize this classification. These determinations are: catechol, acetaldehyde, acetic acid, lactic acid, gaïacol, methyl glyoxal and 3-hydroxypyridine.