Selasa, 31 Januari 2012

Analytical

this is my final assignment in  analytical chemistry. hope that it will be useful for you;D

SEPARATION OF ALKALOID IN JOHAR LEAF’S (Cassia siamea Lamk) USING EXTRACTION

I.            INTRODUCTION
Indonesia is a country with tropical climate. As a consequence, Indonesia has rich and varied flora. Local people have a long tradition of using plants for medicinal purposes and they are still utilising them. However, most of the plants have not been studied chemically and pharmacologically, and there is great potential for the isolation of novel, maturally-occuring bioactive compounds.
The leaves of Cassia siamea Lamk or commonly named by daun johar had been used as plant medicine, especially traditional drug. It is usually used by some people to overcome malaria diseases. Traditional use of Johar leaf againts malaria disease may be effective to kill the malaria parasites. It also can used to wash the injury and incentive the appetite. Based on the research Cassia siamea leaves contain sitosterol, lignin, para kumarat acid, kuinon, and alkaloid (Astuti, 2010).
One kind of separation method can use to separate alkanoid from Johar leaf’s is extraction. Basically, extraction used the difference of solubility of solute in two liquids phase which doesn’t soluble each other. Generally extraction is a attraction process of a solute in its solution in water by the other solvent which doesn’t dissolve in water. In this case, we will separate alkaloid from Johar (Cassia siamea) leaf.  

II.            DESCRIPTION OF STUDY AREA
The leaf of Cassia siamea Lamk usually used by some people to overcome malaria diseases. Traditional use of johar leaf againts malaria disease may be effective to kill the malaria parasites or to reduce fever, because people who are suffering from malaria produce fever. Malaria, caused by parasites of the genus Plasmodium, is one of the leading infectious diseases in many tropical regions (Adebayo and Krettli, 2010). It also can used to wash the injury and incentive the appetite.
Alkaloids have diverse structures and many show a range of pharmacological activities including antimicrobial activity. They are also normally readily separable from the other plant metabolites as a result of their basicity (Hadi and Bremmer, 2001). Almost alkaloid has certain pharmacological reactivity. Some alkaloid is poisoning, and the other is very useful in medical treatment. In human, alkaloid is used to reduce the fever, painful, blood pressure and tumor activity (Henry in Astuti, 2010). In plant, alkaloid is used to metabolism, self protection from insects, parasite, fungi, and bacteri. It also used to reduce or accelerate the growth (Schlitter in Astuti, 2010)
Most of alkaloid has polycyclic skeleton which contain atom C, O, N, H, and the other. This compound can be found in  solid state, amorf, and almost colourless solution. Alkaloid with complex structure and aromatic has colour, like berberine and betanine has yellow colour (Henry in Astuti, 2010).Generally alkaloid is base and soluble in organic solvent. This base properties based on the existence of lone pair in functional group of nitrogen which bond with nitrogen, and it’s aromaticity (Achmad in Astuti, 2010)






                         Picture 1: Molecular structure of alkaloid

III.            METHODE OF EXPERIMENT
Based on the literature, materials and method used is:
A.    Equipments
1.      Beaker glass
2.      Mortar and pestle
3.      Filter paper
4.      Evaporating dish
5.      Oven
B.     Materials
1.      Cassia Senea Lamk leaf
2.      Methanol
3.      Acetic acid 5%
4.      Chloroform
5.      Water(aquades)
6.      Sodium carbonate
C.     Method
1.      100 gram of Johar leaf are grinded by mortar and pestle.
2.      Soak or submerged in methanol.
3.      Filter the filtrate by filter paper
4.      Evaporate in temperature 400C until dry
5.      Dried in oven in temperature 400C as long 48 hours
6.      Added by acetic acid 5% until produce alkaloid salt which is soluble in water, the colour of solution turn brown.
7.      Extract the alkaloid salt by chloroform until get the colourless solution in chloroform, and solution in water phase is brown.
8.      Added sodium carbonate to attract the alkaloid salt until PH is 10 and the colour is red brownish.
9.      Extract again by chloroform until there is no alkaloid in water.
10.  Evaporate the organic solvent (chloroform) until get the brown precipitate.

IV.            DATA ANALYSIS
In the second procedure, we soak or submerged the Johar leaf powder to dissolve all the organic compound contained in this powder in organic compound, methanol. Extract of methanol got is filtered to avoid the big particle of solution. This extract is green brownish. Then we evaporate it in oven and in temperature 400C in order to evaporate the methanol. The temperature is quite low because alkaloid is easy to damage in high temperature. 
The extract contains many organic compound. To separate the organic compound from alkaloid we used acetic acid 5%. Alkaloid will react with acetic acid produce alkaloid salt, and the other organic compound will react with acetic acid to produce organic salt. The colour of solution changes into brown. Alkaloid is polar, so it can soluble in water. The organic salt will soluble in organic compound, so we can separate the organic salt and alkaloid salt by the difference of solubility in water and organic compound.
The organic solvent use to separate the alkaloid salt and organic salt is chloroform. Organic salt will soluble in chloroform, and the alkaloid salt will soluble in water. This extraction is doing several times until the colour in organic phase is colourless, and the colour in water phase is brown. That means all of the organic salt is soluble in chloroform and alkaloid salt soluble in water phase.
To attract the alkaloid from its salt, we add base because adding of base can form pure alkaloid. Base we used is sodium carbonate. We add sodium carbonate until the pH is 10 because most of alkaloid can be extracted in this pH. The colour of this solution is red brownish.
This solution will be extract again by organic solvent. Organic solvent used is chloroform, because alkaloid (not alkaloid salt) will soluble in organic solvent. From the last extraction, we will get the pure alkaloid. After extraction, the organic phase is evaporated in temperature 400C. The alkaloid extract is brown.

V.            CONCLUSION
In this extraction of alkaloid in Johar leaf or Cassia siamea Lamk, we use methanol, chloroform and water as the solvent. Methanol is used to extract all of the organic compound. Chloroform is used to extract the organic salt and pure alkaloid. Water is used to extract the alkaloid salt. Acetic acid is added to produce the organic salt and alkaloid salt which can separate by chloroform. Adding of Sodium carbonate is in order to reach pH 10, so all of pure alkaloid can be attracted from it salt.

VI.            REFRRENCES
Adebayo, J. O., and Krettli, A.U,. 2011. Potential antimalarials from Nigerian Plants: A review. Journal of Ethnopharmacology, vol 133, issue 2, pages 289-302.


Astuti, Yuni. 2010. Isolasi, Identifikasi, dan Karakterisasi Alkaloid dari Kulit Kayu Johar (Cassia siamea Lamk)(pdf).(Online). http://repository.ipb.ac.id/bitstream/handle/123456789/26027/Yuni%20Astuti%20(TM).pdf accesed on 17 december 2011.
Hadi, Surya and Bremmer, John B,. 2001. Initial Studies on Alkaloids from Lombok Medicinal Plants (pdf). Wollongong: Department of Chemistry, University of Wollongong, Australia.
Jumpatong, Kanlaya., Phutdawong, Weerachai., Buddhasukh, Duang. 2006. Dechlorophyllation by Electrocoagulation (pdf). Molecules 2006,11,156-162.
Riza, Fauziyah. Isolation and Identification the chemical Component from Active Mucolytic Fraction of Johar Leaf (Cassia siamea Lamk). Bandung: IPB.

Analytical Coverage

ANALYTICAL COVERAGE

            Analytical chemistry is the science of obtaining, processing, and communicating information about the composition and structure of matter. In the other words, it is the art and science of determining what matter is and how much of it exist.Analytical chemists perform qualitative and quantitaive analysis, use the science of sampling, defining, isolating, concentrating and  preserving samples, set errors limits, validate and verify results through calibration and standarization. They also perform separation by differential chemical properties, create new way to make a measurement, interpret data in proper context and communicate the result.
            Analytical chemistry are employeed in all aspects of chemical research in industry, academia, and government. They do basic laboratory research, develop processes and products, design instruments used in analytical analysis. Teach, and work in marketing and law. Analytical chemistry has many contribution to many fields of science.
1.      Content Analysis
Content analysis is the main section of analytical chemistry. Content analysis will investigate about “what is the component contain in a sample” and “how much the contents present in the sample”. So, we can say that there are two analysis, qualitative analysis and quantitative analysis. Qualitative analysis will give the information about what kind of compound contain in the sample. Quantitative analysis will give information about the quantity of each compound contained in the sample. It also investigate the separation of matter by simple method or classical separation method and some modern separation method using non mechanical engine.Most of the separation is based on physical properties. Some of separation alsoby chemical reaction.
2.      Structural Analysis
Stryuctural analysis is development of question “what is the component contain in a sample”.Stuctural analysis determine by the modern analytical chemistry like mass spectrometry, GC-MS,  LC-MS, and NMR. In this part, we can determine the chemical stucture of chemical uncharacterised substance. We know deeper about the physical and chemical properties of each compound contained in the sample.


3.      Distribution Analysis
Distribution analysis usually used in heterogenous materials. Materials contain more than one substance will have different concentration in every parts of materials. If we know the parts which has highest concentration of certain substances, the separation process will be more efficient in time and work. Beside that, distribution analysis can be described as three dimentional, and the expansion of distribution analysis is on the study of science area. It very useful in develop new material which more useful.
4.      Process Analysis
Processs anlytical chemistry is similar to process analytical technology, it has a origins as a specialized form of analytical chemistry used for process manufacturing. Process analytical chemistry is the aplication of  analytical chemistry with specialized techniques, algorithms, and sampling equipment for solving problems related to chemical processes. The chemical processes are for production abd quality control of manufactured products, and process anlytical technology is used to determine the physical and chemycal properties of the desired products during a manufacturing process.
     Process analysis initially involved sampling the variety of process streams or webs and transporting samples to quality control or central analytical service laboratories. Time delay for analytical results due to sample transport and analytical preparation step negated the value of many chemical analyses for purposes other than product release. Over time it was understood that real-time measurements provided timely information about a process, which was for more useful for high efficiency and quality.The development of development of real-time process amalysis has provided information for process optimization during any manufacturing process.

Source:
David Harvey. Modern Analytical Chemistry. (Pdf).  Accesed in http://www.dr-hanadi.com/upload/Modern.pdf
Wikipedia team. Process Analytical Chemistry. Accesed in http://en.wikipedia.org/wiki/Process_analytical_chemistry

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