NAMA
: IKA SILVI
NIM
: RSA1C110017
PRODI
: PGSBI KIMIA
1. Explain the triterpenoid
biosynthetic pathway, identify important factors that determine the quantities produced many
triterpenoids.
Triterpenoids are a group of mevalonic acid derivative compounds. All types of triterpenoids separated in the same way, ie by TLC and KGC. Identity confirmed
by determining the boiling point.Triterpenoid widespread in resins, coarse, and
kutin plants. Amino
acid triterpenoid resins are often
together with gompolisakarida in amber gum.
Triterpenoids of the most important and widespread are pentacyclic triterpenoids. These compounds are found in plants seprimitif sphagrum, but is most common in seed plants.
Triterpenoids of the most important and widespread are pentacyclic triterpenoids. These compounds are found in plants seprimitif sphagrum, but is most common in seed plants.
On examination triterpenoids
in plants, dry tissue
should be defatted and extracted with hot
methanol. Furthermore, the methanol extract
was hydrolyzed can
be checked directly.
Another detection test used is used for assay detection triterpenoids in general, such as H2SO4 be diluted with water or alcohol.
Another detection test used is used for assay detection triterpenoids in general, such as H2SO4 be diluted with water or alcohol.
2. Describe the structure determination of flavonoids, specificity and intensity
of absorption signal by using
IR and NMR
spectra. Give the
example of at least two different structures.
NMR SPECTRUM of APIGENIN
Infrared spectrum lies in the region with wavelengths
ranging from 0.78 to 1000 nm or wave numbers from 12 800 to 10 cm-7. In terms
of ap, Likasi and instrumentation infrared spectrum is divided into three
types, namely radiation near infrared, mid infrared and far infrared.
Applications are very broad infrared
spectrophotometry for qualitative and quantitative analysis. The applicability of the most is the area of the mid-range wave numbers 4000 to 670
cm-1 or with a
wavelength of 2.3 to 15 μm.
3. In the isolation
of alkaloids, in the early stages
of acid or base required conditions. Explain the
basis of the use of reagents, and give examples
of at least three kinds of alkaloids.
isolation of nicotine
1) 25 grams of chopped dried tobacco leaves that have been wrapped in filter paper inserted into the Soxhlet apparatus, extraction using 300 mL of methanol for 7 hours. The sample used is 100 grams so the extraction is done 4 times.
2) Extract / resulting filtrate evaporated until the resulting solution or filtrate concentrated with 10% of the original volume.
3) concentrated solution is poured into the erlenmeyer flask and acidified with 2 M H2SO4 at 25 mL. The solution was stirred with a magnetic stirer to be homogeneous. The solution was tested with litmus paper to red. Then the solution was extracted with chloroform 25 mL 3 times a separating funnel.
4) Extract the resulting bottom layer is tested with reagents
Dragendorf, if there is a positive alkaloid orange precipitate.
5) The extract was neutralized again by adding NH4OH and then extracted again with 25 mL of chloroform 3 times.
6) The extract obtained was evaporated to aerate, then purified by column chromatography on silica gel 11.5 grams as the stationary phase, column length 10 cm, 3 cm diameter column and eluent n hexane and chloroform, methanol with a ratio of 1:0, 7 : 3, 5:5, 3:7 and 0:1 respectively - each as much as 10 mL.
7) The results of column chromatography followed by thin layer chromatography with a solution of methanol developers.
8) The extract was then tested by using GC-MS, UV-Vis spectrophotometer and IR spectrophotometer.
1) 25 grams of chopped dried tobacco leaves that have been wrapped in filter paper inserted into the Soxhlet apparatus, extraction using 300 mL of methanol for 7 hours. The sample used is 100 grams so the extraction is done 4 times.
2) Extract / resulting filtrate evaporated until the resulting solution or filtrate concentrated with 10% of the original volume.
3) concentrated solution is poured into the erlenmeyer flask and acidified with 2 M H2SO4 at 25 mL. The solution was stirred with a magnetic stirer to be homogeneous. The solution was tested with litmus paper to red. Then the solution was extracted with chloroform 25 mL 3 times a separating funnel.
4) Extract the resulting bottom layer is tested with reagents
Dragendorf, if there is a positive alkaloid orange precipitate.
5) The extract was neutralized again by adding NH4OH and then extracted again with 25 mL of chloroform 3 times.
6) The extract obtained was evaporated to aerate, then purified by column chromatography on silica gel 11.5 grams as the stationary phase, column length 10 cm, 3 cm diameter column and eluent n hexane and chloroform, methanol with a ratio of 1:0, 7 : 3, 5:5, 3:7 and 0:1 respectively - each as much as 10 mL.
7) The results of column chromatography followed by thin layer chromatography with a solution of methanol developers.
8) The extract was then tested by using GC-MS, UV-Vis spectrophotometer and IR spectrophotometer.
Function H2SO4 or concentrated acid is used to facilitate reaching equilibrium or function as katalist
Isolation of kaffein
Tea extract is cooled to room temperature, and then do
the extraction in the funnel by adding 30 ml dichloromethane. Funnel shaken
gently for 5 minutes (so as not to form an emulsion) and the occasional tap
open funnel to reduce the air pressure in the funnel, extraction repeated with
the addition of 30 ml of dichloromethane into a separating funnel,
dichloromethane extract and all the fractions were combined in the form of emulsions
pumpkin erlenmeyer 125 ml, then add calcium chloride anhydrous and emulsion
into the combined extracts, while in the mix and shaken for 10 minutes. Then,
dichloromethane extract was filtered with regular screening. Erlenmeyer and
filter paper rinsed with 5 ml of dichloro methane. Combined filtrate and doing
distillation using a water bath to evaporate the dichloromethane.
The product is weighed and carried rekritalisasi using 5 ml of hot acetone, and the solution was transferred to Pipiet into small erlenmeyer flask. Still in a state of heat, add n-hexane dropwise until turbidity is formed. Refrigerate until it reaches room temperature, then the crystals formed was filtered with suction filtration (vacuum). Crystals washed with a few drops of n-hexane. Then testing the melting point.
Then do the test alkaloids. Crystals of caffeine dissolved in water and etched with 1-2 drops of reagent mayer. If the crystal contains alkaloids, it will form a yellow precipitate. Caffeine crystals are dissolved in water. Then etched with 1-2 drops of Dragendorff reagent. If the crystal contains alkaloids, it will form a precipitate orange.
The product is weighed and carried rekritalisasi using 5 ml of hot acetone, and the solution was transferred to Pipiet into small erlenmeyer flask. Still in a state of heat, add n-hexane dropwise until turbidity is formed. Refrigerate until it reaches room temperature, then the crystals formed was filtered with suction filtration (vacuum). Crystals washed with a few drops of n-hexane. Then testing the melting point.
Then do the test alkaloids. Crystals of caffeine dissolved in water and etched with 1-2 drops of reagent mayer. If the crystal contains alkaloids, it will form a yellow precipitate. Caffeine crystals are dissolved in water. Then etched with 1-2 drops of Dragendorff reagent. If the crystal contains alkaloids, it will form a precipitate orange.
Caffeine used in
isolation reagent dichloromethane dichloromethane which is where it functions
to dissolve nonpolar substances bound bully so pure caffeine and can be
extracted
a. Pretreatment
Slobber fresh leaves taken from the trunk, separated from the plants that are less good, sorted, cut into small pieces and then dibelender until smooth and dried without exposure to direct sunlight.
b. Extraction Method
The leaves have smooth slobber weighed as much as 200, after which macerated with petroleum ether 1 x 24 hours, then the residue was macerated with 10% acetic acid in 96% ethanol for 3 x 24 hours in the ratio 1: 3. The extract obtained was concentrated by evaporator to about a quarter of the initial volume. The ethanol extract obtained concentrated ammonium hydroxide solution is added 10% by way of drop little by little, to precipitate alkaloids. The precipitate obtained was washed with ammonium hydroxide 10% and direkristakisasi using chloroform.
Slobber fresh leaves taken from the trunk, separated from the plants that are less good, sorted, cut into small pieces and then dibelender until smooth and dried without exposure to direct sunlight.
b. Extraction Method
The leaves have smooth slobber weighed as much as 200, after which macerated with petroleum ether 1 x 24 hours, then the residue was macerated with 10% acetic acid in 96% ethanol for 3 x 24 hours in the ratio 1: 3. The extract obtained was concentrated by evaporator to about a quarter of the initial volume. The ethanol extract obtained concentrated ammonium hydroxide solution is added 10% by way of drop little by little, to precipitate alkaloids. The precipitate obtained was washed with ammonium hydroxide 10% and direkristakisasi using chloroform.
In isolation leaves slobber use ethanol,
which works to attract alkaloid compounds thus obtain the desired extract
4. Describe the relationship between biosynthesis, methods of isolation and structural determination of
compounds Give examples of natural materials.
The first Addisi Mannich reaction,
ie enolate anion from acetyl-CoA acting as
a nucleophile to cation pyrrolinium. Addisi both going through Claisen condensation produces a
racemic mixture of 2-substituted
pyrrolidine.
Biosynthetic functions is that we can know the reaction
of the compound of cocaine, knowing that the resulting compound, then we can
multiply these compounds by means of isolation or insulation aims to find the
desired compounds in a sample and reproduced, then after we sampled the
mengetahuia if there is a compound of cocaine then the next step is to identify
compounds that cocaine with IR spectroscopy and NMR spectroscopy in which we
can find out where the group of cocaine by looking at wavelengths appear around
the area. Thus the biosynthesis, isolation and identification of a compound
closely related if we want to get a desired compound
