CERTIFICATE OF ANALYSIS - GC PROFILING

Transcription

1 Date : April 25, 2018 CERTIFICATE OF ANALYSIS - GC PROFILING SAMPLE IDENTIFICATION Internal code : 18D18-HBN4-1-CC Customer identification : Tea Tree Oil Type : Essential oil Source : Melaleuca alternifolia ct. Terpinen-4-ol Customer : Health & Beauty Natural Oils ANALYSIS Method: PC-PA J19 - Analysis of the composition of an essential oil, or other volatile liquid, by FAST GC-FID (in French); identifications validated by GC-MS. Analyst : Sylvain Mercier, M. Sc., Chimiste Analysis date : April 20, 2018 Checked and approved by : Alexis St-Gelais, M. Sc., chimiste Note: This report may not be published, including online, without the written consent from Laboratoire PhytoChemia. This report is digitally signed, it is only considered valid if the digital signature is intact. Page 1/12

2 PHYSICOCHEMICAL DATA Physical aspect: Clear liquid Refractive index: ± (20 C) COMPLIANCE WITH ISO 4730:2017 (OIL OF MELALEUCA, TERPINEN-4-OL TYPE (TEA TREE OIL)) Compound Prescribed content Min. % Max. % Observed % Complies? α-pinene Yes Sabinene tr Yes α-terpinene Yes Limonene Yes para-cymene Yes 1,8-Cineole tr Yes γ-terpinene Yes Terpinolene Yes Terpinen-4-ol Yes α-terpineol Yes Aromadendrene Yes Viridiflorene Yes δ-cadinene Yes Globulol tr Yes Viridiflorol tr Yes Refractive index Yes CONCLUSION No adulterant, contaminant or diluent has been detected using this method. The oil complies with the ISO standard for tea tree oil. Page 2/12

3 ANALYSIS SUMMARY Identification DB-5 (%) DB-WAX (%) Classe Ethanol Aliphatic alcohol Isobutyral Aliphatic aldehyde Ethyl acetate 0.01 tr Aliphatic ester Isobutanol tr 0.70* Aliphatic alcohol Isovaleral tr tr Aliphatic aldehyde 2-Methylbutyral Aliphatic aldehyde Isoamyl alcohol tr tr* Aliphatic alcohol 2-Methylbutanol tr [tr]* Aliphatic alcohol Isobutyric acid tr Aliphatic acid (3Z)-Hexenol Aliphatic alcohol Hexanol tr 0.01 Aliphatic alcohol α-thujene Monoterpene α-pinene Monoterpene Camphene 0.02* 0.01 Monoterpene α-fenchene [0.02]* tr Monoterpene Thuja-2,4(10)-diene tr 0.27* Monoterpene Sabinene 0.97* [0.27]* Monoterpene β-pinene [0.97]* [0.70]* Monoterpene 3-Methyl-3-cyclohexenone? * Aliphatic ketone Myrcene Monoterpene Pseudolimonene 0.51* 0.01 Monoterpene α-phellandrene [0.51]* 0.51 Monoterpene (3Z)-Hexenyl acetate Aliphatic ester α-terpinene Monoterpene Carvomenthene Aliphatic alcohol para-cymene Monoterpene β-phellandrene 3.57* 1.00 Monoterpene Limonene [3.57]* 0.80 Monoterpene 1,8-Cineole [3.57] 1.72 Monoterpenic ether (Z)-β-Ocimene * Monoterpene (E)-β-Ocimene Monoterpene γ-terpinene [19.67]* Monoterpene cis-sabinene hydrate Monoterpenic alcohol Terpinolene Monoterpene trans-sabinene hydrate Monoterpenic alcohol Linalool Monoterpenic alcohol Unknown * Monoterpenic alcohol para-mentha-1,3,8-triene 0.01 [0.02]* Monoterpene cis-para-menth-2-en-1-ol Monoterpenic alcohol 4-Hydroxy-4-methylcyclohex-2-enone Aliphatic alcohol Cosmene isomer I 0.18* 0.06 Monoterpene trans-para-menth-2-en-1-ol [0.18]* 0.80* Monoterpenic alcohol Unknown * Unknown Borneol * Monoterpenic alcohol δ-terpineol tr 0.01 Monoterpenic alcohol Terpinen-4-ol 39.24* 39.12* Monoterpenic alcohol Dill ether [39.24]* tr Monoterpenic ether para-cymen-8-ol [39.24] 0.05 Monoterpenic alcohol Page 3/12

4 α-terpineol 2.91 [3.03]* Monoterpenic alcohol cis-piperitol Monoterpenic alcohol Unknown 0.02 Oxygenated monoterpene trans-piperitol Monoterpenic alcohol endo-fenchyl acetate 0.01 [0.16]* Monoterpenic ester exo-2-hydroxycineole Monoterpenic alcohol Nerol Monoterpenic alcohol Piperitone Monoterpenic ketone cis-carvenone oxide? 0.02 Monoterpenic ketone trans-ascaridole glycol Monoterpenic alcohol cis-ascaridole glycol? Monoterpenic alcohol Thymol Monoterpenic alcohol Carvacrol Monoterpenic alcohol Unknown Monoterpenic alcohol Bicycloelemene Sesquiterpene α-cubebene Sesquiterpene Isoledene 0.07 [0.16]* Sesquiterpene α-copaene Sesquiterpene 7-Cubebene 0.07* 0.07 Sesquiterpene 7-Cubebene epimer? [0.07]* 0.03 Aliphatic alcohol β-cubebene Sesquiterpene β-elemene 0.04 [1.33]* Sesquiterpene α-gurjunene Sesquiterpene β-maaliene Sesquiterpene β-caryophyllene Sesquiterpene γ-maaliene Sesquiterpene β-gurjunene Sesquiterpene α-maaliene 0.08 [39.12]* Sesquiterpene Aromadendrene 1.40 [1.33]* Sesquiterpene Selina-5,11-diene Sesquiterpene trans-muurola-3,5-diene Sesquiterpene α-humulene Sesquiterpene allo-aromadendrene 0.64* [0.80]* Sesquiterpene Valerena-4,7(11)-diene [0.64]* 0.02 Sesquiterpene γ-gurjunene Sesquiterpene trans-cadina-1(6),4-diene 0.39* 0.35 Sesquiterpene Selina-4,11-diene [0.39]* 0.03 Sesquiterpene γ-muurolene Sesquiterpene β-selinene Sesquiterpene allo-aromadendr-9-ene Sesquiterpene trans-muurola-4(15),5-diene 0.10 [3.03]* Sesquiterpene δ-selinene * Sesquiterpene Viridiflorene 2.13* [1.20]* Sesquiterpene Bicyclogermacrene [2.13]* 0.95 Sesquiterpene α-selinene [2.13]* 0.03 Sesquiterpene α-muurolene Sesquiterpene γ-cadinene 0.04 [1.82]* Sesquiterpene trans-calamenene Sesquiterpene Zonarene 1.74* [1.82]* Sesquiterpene δ-cadinene [1.74]* [1.82]* Sesquiterpene trans-cadina-1,4-diene Sesquiterpene α-calacorene Sesquiterpene Page 4/12

5 Eudesma-5,7(11)-diene Sesquiterpene Unknown Oxygenated sesquiterpene Spathulenol Sesquiterpenic alcohol Globulol Sesquiterpenic alcohol Gleenol Sesquiterpenic alcohol Viridiflorol Sesquiterpenic alcohol Cubeban-11-ol * Sesquiterpenic alcohol Ledol 0.15* 0.06 Sesquiterpenic alcohol Eudesm-5-en-11-ol analog [0.15]* 0.09 Sesquiterpenic alcohol 10-epi-Cubenol 0.01 Sesquiterpenic alcohol Rosifoliol Sesquiterpenic alcohol 1-epi-Cubenol Sesquiterpenic alcohol Isospathulenol Sesquiterpenic alcohol Cubenol 0.13 [0.26]* Sesquiterpenic alcohol α-muurolol Sesquiterpenic alcohol Total identified 98.72% 98.73% *: Two or more compounds are coeluting on this column [xx]: Duplicate percentage due to coelutions, not taken account in the identified total tr: The compound has been detected below 0.005% of total signal. Note: no correction factor was applied Page 5/12

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9 FULL ANALYSIS DATA Identification Column DB-5 Column DB-WAX R.T R.I % R.T R.I % Ethanol Isobutyral Ethyl acetate tr Isobutanol tr 2.13* Isovaleral tr tr 2-Methylbutyral Isoamyl alcohol tr 3.45* 1175 tr 2-Methylbutanol tr 3.45* 1175 [tr] Isobutyric acid tr (3Z)-Hexenol Hexanol tr α-thujene α-pinene Camphene 3.19* α-fenchene 3.19* 940 [0.02] tr Thuja-2,4(10)- diene tr 2.31* Sabinene 3.61* * 1088 [0.27] β-pinene 3.61* 968 [0.97] 2.13* 1070 [0.70] 3-Methyl-3- cyclohexenone? * Myrcene Pseudolimonene 4.06* α-phellandrene 4.06* 999 [0.51] (3Z)-Hexenyl acetate α-terpinene Carvomenthene para-cymene β-phellandrene 4.44* Limonene 4.44* 1023 [3.57] ,8-Cineole [3.57] (Z)-β-Ocimene * (E)-β-Ocimene γ-terpinene * 1207 [19.67] cis-sabinene hydrate Terpinolene trans-sabinene hydrate Linalool Unknown [m/z 119, 109 (94), 43 (61), 95 (56), 91 (48), 77 (32), * (32), 137 (31), 134 (24)] para-mentha-1,3, * 1375 [0.02] Page 9/12

10 Borneol * δ-terpineol tr Terpinen-4-ol 6.84* * Dill ether 6.84* 1176 [39.24] tr para-cymen-8-ol [39.24] α-terpineol * 1655 [3.03] cis-piperitol Unknown [m/z 121, 43 (99), 91 (85), 77 (73), 93 (41), 136 (33) (3)] triene cis-para-menth-2- en-1-ol Hydroxy-4- methylcyclohex enone Cosmene isomer I 6.20* trans-para-menth- 2-en-1-ol 6.20* 1135 [0.18] 9.04* Unknown [m/z 109, 124 (45), 119 (41), 43 (35), 91 (28), 95 (25)...] * trans-piperitol endo-fenchyl acetate * 1425 [0.16] exo-2- Hydroxycineole Nerol Piperitone cis-carvenone oxide? trans-ascaridole glycol cis-ascaridole glycol? Thymol Carvacrol Unknown [m/z 97, 112 (92), 83 (62), 43 (44), 41 (25) ? (4)] Bicycloelemene α-cubebene Isoledene * 1425 [0.16] α-copaene Cubebene 9.72* Cubebene epimer? 9.72* 1372 [0.07] β-cubebene Page 10/12

11 β-elemene * 1555 [1.33] α-gurjunene β-maaliene β-caryophyllene γ-maaliene β-gurjunene α-maaliene * 1562 [39.12] Aromadendrene * 1555 [1.33] Selina-5,11-diene trans-muurola-3,5- diene α-humulene allo- Aromadendrene 10.80* * 1589 [0.80] Valerena-4,7(11)- diene 10.80* 1452 [0.64] γ-gurjunene trans-cadina- 1(6),4-diene 11.00* Selina-4,11-diene 11.00* 1467 [0.39] γ-muurolene β-selinene allo-aromadendr- 9-ene trans-muurola- 4(15),5-diene * 1655 [3.03] δ-selinene * Viridiflorene 11.28* * 1641 [1.20] Bicyclogermacrene 11.28* 1488 [2.13] α-selinene 11.28* 1488 [2.13] α-muurolene γ-cadinene * 1704 [1.82] trans-calamenene Zonarene 11.67* * 1704 [1.82] δ-cadinene 11.67* 1518 [1.74] 10.46* 1704 [1.82] trans-cadina-1,4- diene α-calacorene Eudesma-5,7(11)- diene Unknown [m/z 161, 109 (98), 82 (93), 43 (72), 105 (68), 93 (59), (56), 119 (55) (7)] Spathulenol Globulol Gleenol Viridiflorol Cubeban-11-ol * Ledol 12.61* Page 11/12

12 Eudesm-5-en-11-ol analog 12.61* 1592 [0.15] epi-Cubenol Rosifoliol epi-Cubenol Isospathulenol Cubenol * 1994 [0.26] α-muurolol Total identified 98.72% 98.73% Total reported 99.00% 98.87% *: Two or more compounds are coeluting on this column [xx]: Duplicate percentage due to coelutions, not taken account in the identified total : Peaks apexes were resolved, but peaks overlapped and were summed for analysis tr: The compound has been detected below 0.005% of total signal. Note: no correction factor was applied R.T.: Retention time (minutes) R.I.: Retention index Page 12/12