Characterization and Determination of Percentage of Carvone in the Spearmint Oil by Using GLC

 

Preeti Jain* and Jeetendra Bhawsar

Department of Chemistry, Medi-Caps Institute of Technology and Management, Indore (M.P)

*Corresponding Author E-mail: preetijain278@gmail.com

ABSTRACT:

In the present study physical characteristics and percentage of carvone were determined in spearmint oil. The Specific gravity was 0.920 to 0.940 (0.914 to 0.934 at 25°); rotation was 36° to- 50°. Soluble in its own volume of alcohol (95 per cent.), forming a clear solution; also soluble in all proportions of absolute alcohol, and in about its own volume of alcohol (90 per cent.), the solution becoming opalescent on adding more solvent. The chief constituent of the oil was carvone. Boiling-point was 230°C. It is an unsaturated ketone, having the formula C₁₀H₁₄O, and is a colourless liquid, smelling strongly of caraway, and solidifying on refrigeration. The chromatogram obtained by GLC type NUCON 5700 (Gas liquid chromatography) depicted that the percentage of carvone in the oil sample was 82 % concluding that its effectiveness was more than other oil.

 

 

 

INTRODUCTION:

Spearmint oil is extracted by steam distilling the flowering tops. The main chemical components of Spearmint oil are Carvone, Cineole, Limonene, Myrcene, Phellandrene and Caryophyllene. It is non-toxic, non-irritant and non-sensitizing¹. Spearmint oil can be effective for the digestive system, for the respiratory tract, for a tired mind and for skin problems. The therapeutic properties of spearmint oil are local anesthetic, antispasmodic, astringent, carminative, decongestant, digestive, diuretic, expectorant, stimulant and restorative. Spearmint oil could be helpful with digestive problems like vomiting, flatulence, constipation, colic and dyspepsia. It stimulates a tired mind and helps with headaches, migraines, nervous strain, fatigue and stress. For the respiratory tract Spearmint oil could help with asthma, bronchitis, catarrh and sinusitis. It can relieve the itching of pruritus; and helps with acne, dermatitis, congested skin and sore gums.

 

Spearmint oil blends well with any oil, it blends particularly well with Basil, Eucalyptus, Lavender, Rosemary and Jasmine. Oil of spearmint (Oleum Menthae; Oleum Menthae Crispae) is obtained by distillation from fresh, flowering spearmint, Mentha viridis and M. crispa, a native of Europe and Asia, cultivated for domestic use as well as for the sake of its oil, most of which is imported from America.

 

Oil of spearmint occurs as a colourless, pale yellow or greenish-yellow liquid when distilled, but becomes darker and viscid on keeping; it has the characteristic odour, and warm slightly bitter taste of the spearmint, the taste being less pungent than that of peppermint¹. Carvone is a member of a family of chemicals called terpenoids². Carvone is found naturally in many essential oils, but is most abundant in the oils from seeds of caraway (Carum carvi) and dill^3,4. Carvone is used in the food and flavor industry. L-(-)-Carvone is also used for air freshening products and, like many essential oils, oils containing carvones are used in aromatherapy and alternative medicine^3,4.

 

METHODS AND MATERIAL:

A chromatogram of spearmint oil is determined .The details are as follows.

1)      Set the column flow rate of carrier gas supply.

2)      Switch the mains of temperature controller module.

3)      Set the oven temperature to the required minimum temperature.

4)      Switch on the injector and detector (FID) heater and set the dial of injector and detector controller for the required temperature.

5)      Allow the system to stabilize

6)      Set different parameter such as attenutator, sensitivity, programming rate etc.

7)      Light flame in the detector.

8)      Liquid sample can be injected through injection port by piercing a septum on the injector port via a micro liter syringe

 

Table 1: Spearmint-80 GLC Results

R.TIME	HEIGHT	AREA	HT%	AREA%	TYPE	AR/HT
1.73	222	6460	0.4537	0.0461	BV	0.020
1.78	545	15786	1.1139	0.1125	VB	0.019
3.86	-	5354	--	0.0382	BP	0.034
4.34	--	6204	--	0.0442	BV	0.041
4.43	276	14936	0.5641	0.1065	VV	0.037
4.51	268	14134	0.5478	0.1008	VV	0.036
4.56	427	25889	0.8727	0.1846	VP	0.041
4.81	148	11932	0.3025	0.0851	PV	0.055
4.97	129	8364	0.2637	0.0596	VV	0.044
5.09	863	65393	1.7639	0.4663	VV	0.052
5.31	14445	1250511	29.5242	8.9163	VP	0.059
5.56	--	3076	--	0.0219	TTT	0.047
5.80	--	9513	--	0.0678	PV	0.061
6.14	--	2272	--	0.0162	VV	0.260
6.30	--	2724	--	0.0194	VV	0.055
6.44	--	5825	--	0.0415	VV	0.051
6.54	--	4620	--	0.0329	VB	0.127
7.30	--	5814	--	0.0414	BV	0.129
7.72	1421	157157	2.9044	1.1205	VV	0.076
7.95	1750	163910	3.5768	1.1687	VV	0.064
8.18	1730	213934	3.5359	1.5254	VV	0.085
8.37	1864	292568	3.8098	2.0861	VV	0.108
8.65	408	92937	0.8337	0.6626	VB	0.156
10.49	24430	.11538377E08	49.9325	82.2705	BB	0.325
10.67	--	5361	--	0.0382	TTP	0.051
10.93	--	6763	--	0.0482	TPP	0.068
11.11	--	3357	--	0.0239	TPV	0.096
11.24	--	4357	--	0.0311	TVV	0.096
11.87	--	12188	--	0.0869	TVT	0.90
12.31	--	4183	--	0.0298	TTP	0.143
12.57	--	11231	--	0.0801	TPV	0.080
12.92	--	5031	--	0.0359	TVT	0.080
13.45	--	4105	--	0.0293	BV	0.148
13.94	--	11969	--	0.0853	VB	0.092
14.52	--	3818	--	0.0272	BV	0.082
14.63	--	3290	--	0.0234	VB	0.080
15.06	--	4451	--	0.0317	BP	0.069
15.58	--	2227	--	0.0159	PB	0.069
16.11	--	16726	--	0.1192	BV	0.095
17.11	--	4300	--	0.0306	VB	0.113
23.23	--	3863	--	0.0275	BB	0.126

 

Fig.1

 

9)      Use programming mode

10)   With the help of recorder record the components detected by the detector i.e Qualitative and quantitative analyses

11)   When recording is completed switching off in sequence

12)   Switch off the recorder and close the hydrogen shut off value the flames will go off, and then shut off air supply.

13)   Switch off injector heating power.

14)   Allow the temperature of the oven and  detector to almost ambient temperature

15)   Stop the carrier gas only when the column and detector temperature has fallen to near ambient temperature.

 

EXPERIMENT:

GLC Type-             NUCON-5700

Column -               Supelco – 24319

30 M Multiplied by 0.32 m

Film 0.2 mum

Coloumn # 11468-078

Carrier Gas            N₂ Pressure 4 kg/cm²

Which Splits into two Columns each having 2 kg/cm² Pressure

H₂ Pressure 0.8 kg/cm²

O₂ Pressure 1 kg/cm²

Parameters

Sensitivity    - 100 X

Attenuation – 4X

Oven Initial Temperature     – 90 Degree

Oven Final Temperature      – 260 Degree

Injector Temperature                           – 280 Degree

Detector Temperature                         – 280 Degree

Chromatogram is of Spearmint Oil 80 %

Contains 82% CARVON

 

RESULT AND DISCUSSION:

The chief constituent of the oil under examination was carvone, Boiling-point, 230°.C Specific gravity, 0.964. It is an unsaturated ketone, having the formula C₁₀H₁₄O, and is a colourless liquid, smelling strongly of caraway, and solidifying on refrigeration. It’s combined with hydrogen sulphide to form a crystalline addition compound, but not with bisulphites. The constituent to which the odour of the oil is attributed is said to be the acetic ester of dihydrocuminol⁵. The chromatogram obtained (Fig.-1) by GLC Nucon and observation (Table-1) shows that the percentage of carvone in the oil sample of spearmint oil was 82 % concluding that its effectiveness is more than other oil.

 

REFERENCES:

1.       http://www.aromatherapy-oil.co.uk/spearmint.htm [Link]

2.       Simonsen, J. L. (1953). The Terpenes. 1 (2nd ed.). Cambridge: Cambridge University Press. pp. 394–408.

3.       De Carvalho, C. C. C. R; Da Fonseca, M. M. R. "Carvone: Why and how should one bother to produce this terpene" Food Chemistry 2006, 95, 413-422.

4.       http://en.wikipedia.org/wiki/Carvone [Link]

5.       http://www.henriettesherbal.com/eclectic/bpc1911/mentha-viri_oleu.html [Link]

 

 

Received on 27.08.2010        Modified on 15.09.2010

Accepted on 22.09.2010        © AJRC All right reserved