Houessou, Justin Koffi (2007) Polycyclic aromatic hydrocarbons in coffee : development of analytical methods and study of the roasting process. PhD thesis Chimie analytique, Chimie analytique, AgroParistech 2007AGPT0002 p.175.

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Table of content

INTRODUCTION - 1

1 LE CAFÉ - 4

1.1 PRÉSENTATION DU CAFÉ - 4

1.1.1 Un produit très consommé - 4

1.1.2 Le commerce du café - 5

1.1.3 Les variétés de café - 5

1.1.4 La production des grains de café - 6

1.1.5 La production du café moulu et de sa boisson - 13

1.2 COMPOSITION DU CAFÉ - 16

1.2.1 La composition des grains de café vert - 17

1.2.2 La composition des grains de café torréfiés - 27

1.2.3 La composition du café boisson - 37

1.2.4 Conclusion sur la composition du café - 41

1.3 LES EFFETS PHYSIOLOGIQUES DU CAFÉ BOISSON - 41

1.3.1 Les effets bénéfiques pour la santé - 41

1.3.2 Les effets préjudiciables pour la santé - 44

1.4 LES HYDROCARBURES AROMATIQUES POLYCYCLIQUES DANS LE CAFÉ - 46

1.4.1 Les teneurs en HAP de divers cafés - 46

1.4.2 Les procédures analytiques mises en oeuvre - 50

1.4.3 Les sources de contamination du café par les HAP - 51

1.4.4 Conclusion sur les HAP dans le café - 57

2 MATERIELS ET METHODES - 60

2.1 PRODUITS ET RÉACTIFS - 60

2.1.1 Solvants - 60

2.1.2 Standards et réactifs - 60

2.1.3 Matériel utilisé pour l’extraction en phase solide - 61

2.1.4 Cafés étudiés - 62

2.2 MÉTHODES DE TRAITEMENT DES ÉCHANTILLONS DE CAFÉ BOISSON - 62

2.2.1 Procédure de préparation du café boisson - 62

2.2.2 Extraction en phase solide directe du café boisson - 63

2.2.3 Saponification préalable du café boisson - 64

2.3 MÉTHODES DE TRAITEMENT DES ÉCHANTILLONS DE CAFÉ MOULU - 65

2.3.1 Mise en oeuvre de l’extraction accélérée par solvant - 66

2.3.2 Mise en oeuvre de l’extraction par Soxhlet - 73

2.3.3 Mise en oeuvre d’une saponification alcaline directe - 74

2.4 TORRÉFACTION DES ÉCHANTILLONS DE CAFÉ VERT - 75

2.5 MÉTHODES ANALYTIQUES - 76

2.5.1 Analyse quantitative des HAP par HPLC-FD - 77

2.5.2 Analyse qualitative des HAP par HPLC-UV-DAD - 77

2.5.3 Identification des HAP par GC-MS/MS et analyse semi-quantitative - 78

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3 MISE AU POINT DE PROCÉDURES ANALYTIQUES POUR LA

DÉTERMINATION DES HAP DANS LE CAFÉ - 84

3.1 DÉTERMINATION DES HAP DANS LE CAFÉ MOULU - 84

3.1.1 Choix d’une méthode de purification de l’extrait PSE - 84

3.1.2 Choix des conditions de mise en oeuvre de l’extraction PSE - 95

3.1.3 Intérêt de la mise en oeuvre d’une extraction PSE - 100

3.1.4 Evaluation des performances de la méthode - 104

3.1.5 Application à la détermination des HAP dans divers cafés moulus - 105

3.2 DÉTERMINATION DES HAP DANS LE CAFÉ BOISSON - 114

3.2.1 Optimisation des conditions d’extraction en phase solide - 114

3.2.2 Mise en oeuvre de la méthode SPE retenue - 126

3.2.3 Etude de la mise en oeuvre d’une étape de saponification - 132

3.2.4 Conclusion - 134

3.3 ESTIMATION DES COEFFICIENTS DE TRANSFERT DES HAP DU CAFÉ MOULU VERS LE

CAFÉ BOISSON - 134

3.4 CONCLUSION - 136

4 INFLUENCE DE LA TORREFACTION SUR LA PRESENCE DES HAP DANS

LE CAFE - 138

4.1 INTRODUCTION - 138

4.2 ETUDE DES CONDITIONS DE TORREFACTION SUR LA TENEUR EN HAP DU CAFE MOULU

- 138

4.2.1 Infuence de la durée de torréfaction à 260°C - 139

4.2.2 Infuence de la température de torréfaction à durée constante - 151

4.2.3 Modélisation avancée de la formation des HAP - 161

4.2.4 Confirmation de la présence des HAP dans les cafés torréfiés - 169

4.2.5 Conclusion - 172

4.3 ETUDE DES CONCENTRATIONS EN HAP DES CAFES BOISSONS - 172

4.3.1 Analyse des cafés boissons préparés à partir de cafés torréfiés pendant 5 min172

4.3.2 Analyse des cafés boissons préparés à partir de cafés torréfiés pendant 20 min174

4.3.3 Estimation des coefficients de transfert des HAP - 175

4.3.4 Conclusion sur le café boisson - 177

4.4 CONCLUSION - 178

CONCLUSIONS ET PERSPECTIVES - 180

RÉFÉRENCES BIBLIOGRAPHIQUES - Référence 183

ANNEXES

ANNEXE 1 : Les composés volatils extraits du café torréfié par HS-SPME

ANNEXE 2 : Structures chimiques et propriétés des 16 HAP classés polluants prioritaires par

l’US EPA

ANNEXE 3 : Les HAP et leur toxicité

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ANNEXE 4: LA CHROMATOGRAPHIE LIQUIDE HAUTE PERFORMANCE COUPLEE

A UN DETECTEUR DE FLUORESCENCE

ANNEXE 5 : LA CHROMATOGRAPHIE LIQUIDE HAUTE PERFORMANCE COUPLEE

A UN DETECTEUR UV

ANNEXE 6 : LA CHROMATOGRAPHIE EN PHASE GAZEUSE COUPLEE A LA

SPECTROMETRIE DE MASSE

ANNEXE 7 : EVALUATION DU POTENTIEL TOXIQUE DU MELANGE DES HAP

ANNEXE 8 : IDENTIFICATION DES HAP DANS LES CAFES MOULUS DU

COMMERCE PAR GC-MS/MS

ANNEXE 9 : ETUDE DE LA CINETIQUE DE FORMATION DES HAP

ANNEXE 10 : MODELISATION DE LA FORMATION DES HAP A L’AIDE D’UN

RESEAU DE NEURONES

ANNEXE 11 : IDENTIFICATION DES HAP DANS LES CAFES MOULUS TORREFIES

PAR GC-MS/MS

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