EXPERIMENT 10: QUALITATIVE ANALYSIS OF ”DAUN KESUM”

BY GAS CHROMATOGRAPHY- MASS SPECTROMETRY (GC-MS)

NAME: NADIRAH BINTI ZAKARIA

ID: 2016586557

PARTNERS’ NAME:

1. NUR SYAZWANI BINTI MUHAMMAD YAZID (2016596153)

2. SITI ZAHARIAH BINTI ZAHARUDIN (2016552077)
3. WAN NURUL IHSAN BINTI WAN ZAINUDDIN (2016552007)

DATE EXPERIMENT CONDUCTED: 7 JUNE 2017

DATE EXPERIMENT SUBMITTED: 19 JUNE 2017

LECTURER: MADAM ROHAIZA MOHAMAD

 Experiment 10: Qualitative Analysis of “DAUN KESUM” Herb By Gas Chromatography- Mass

Spectrometry (GC-MS)

Objective:

1. To perform an extraction of ”daun kesum” by liquid-liquid extraction.

2. To analyze and identify constituents in the essential oil of ”daun kesum” by using GC/MS.

Introduction:

”Daun kesum” is an herb that useful in producing medicine and oil by using its leaves and oils.

”Daun kesum” also can be used for treating digestive disorder such as indigestion, nausea and diarrhea.

Some people used it for sore throat and headaches. In foods and beverages, ”daun kesum” also used in

the food industry as a general spice and can be found in ice cream, beverages, baked goods, and

condiments. It is used in many foods, and contributes a strong dry wood, pepper, and earthy spice

flavor.

Gas chromatography, specifically gas-liquid chromatography involves a sample being vaporized

and injected onto the head of the chromatographic column. The sample is transported through the

column by the flow of inert, gaseous mobile phase. The column itself contains a liquid stationary phase

which is adsorbed onto the surface of an inert solid. Efficient separation of compounds in GC is

dependent on the compounds travelling through the column at different rates. The rate at which a

compound travels through a particular GC system depends on several factors that include; volatility of

compound, column temperature, carrier gas flow rate and length of the column. In volatility of

compound, low boiling components will travel faster through the column than high boiling components.

In column temperature, raising the column temperature speeds up all the compounds in a mixture. In

carrier gas flow rate, increasing the carrier gas flow rate increase the speed with which all compounds
move through the column. The longer the column, the longer it will take for all compounds to elute.

Longer columns are employed to obtain better separation.

Liquid – liquid extraction is known as solvent extraction and partitioning is a method to separate

compounds based on their relative solubility in two different immiscible liquids such as water and

organic solvent used in experiment. It is also an extraction of a substance from one liquid to another

liquid phase. Liquid – liquid extraction is a basic technique in chemical laboratories where it is

performed using a separatory funnel.

Chemical:

Methanol, Dichloromethane and Anhydrous magnesium sulphate.

Sample: Fresh “daun kesum” leaves.

Apparatus:

Separatory funnel, round bottom flask, vial, dropper and beaker.

Procedure:

1. The “daun kesum” is weighed about 3 – 4 g and recorded.

2. Then, the “daun kesum” is chopped into small pieces and put into round bottom flask.

3. 25 ml of methanol is added to the flask and reflux for about 30 minutes.

4. Then, the solution is poured into separating funnel and 5 ml of dichloromethane is added.

5. After the mixture is shaking vigorously, the organic layer is taken and added with anhydrous

magnesium sulphate.

6. The mixture is filtered by using separating funnel and filtered the final product using syringe

filter to remove any particulate matter and put into vial for analysis using GC.
Results:
Discussion:

After adding 5 ml of dichloromethane, the mixture will form two layers. The upper layer is oil in

brown color and the bottom layer is green in color. Based on the results above, there are present of

caryophyllene in the sample of “daun kesum” which is about 99% quality.

Caryophyllene is a natural bicyclic sesquiterpene that is a constituent of many essential oils

especially clove oil, the oil from the stems and flowers of Syzygium aromaticum (cloves), the essential oil

of Cannabis sativa,rosemary and hops. Caryophyllene is a sesquiterpinoid that comes in two forms

(alpha and beta) which are generally found together (isocaryphollene). It’s a hydrocarbon, and much like

myrcene is widely used in the perfume industry. Caryophyllene is also used in the food industry as a

general spice and can be found in ice cream, beverages, baked goods, and condiments. Caryophyllene

also is used in many foods, and contributes a strong dry wood, pepper, and earthy spice flavor. It is a

colorless to pale yellow liquid and tones of citrus may come to the finish.

When conducting this experiment, there are so many compounds that can be detected such as

decanal, 1,2,3-Benzenetroil, bicyclo 7.2.0 undec-4-ene 4 11 11-trimethyl-8-methylene- and many more.

These compounds were analyzed using GC-MS. From the analysis data, we can determine the name of

compounds presented in the sample by referring to the list of compounds in the library of GC-MS

instrument.

Conclusion:

As the conclusion, “daun kesum” was extracted by using liquid-liquid extraction and the constituent of
the “daun kesum” is determined. We also can conclude that many compounds that contribute to the
“daun kesum” leaves including caryophyllene and menthol.
References:

1. Analytical separation methods laboratory guide: 2nd edition. Nor’ashikin Saim, Ruziyati Tajuddin

and Mardiana Saaid. (2016)

2. Caryophyllene. Retrieved Jun 18, 2017 from https://en.wikipedia.org/wiki/Caryophyllene

3. Caryophyllene oil. Retrieved Jun 18, 2017 from http://beerlegends.com/caryophyllene-oil