GUIDE BOOK
PRACTICAL OF QUALITATIVE
PHARMACEUTICAL CHEMISTRY
YADE METRI PERMATA, S.Farm., M.Si., Apt. Dra. TUTY ROIDA PARDEDE, M.Si., Apt.
Prof.Dr. MASFRIA, M.S., Apt. Prof.Dr. MUCHLISYAM, M.Si., Apt.
LISDA RIMAYANI NASUTION, S.Farm., M.Si., Apt.
QUALITATIVE PHARMACEUTIAL CHEMISTRY LABORATORY
FACULTY OF PHARMACY
UNIVERSITY OF SUMATERA UTARA
MEDAN
2020
2
PREFACE
This guidebook is compiled to make it easier for students to do practice about the
identification of various medicinal ingredients quickly in a chemical reaction according
to our experience in the Qualitative Pharmaceutical Chemistry Laboratory.
This book can be used as a guide for students in identification of chemical drug
conventionally. Although with the technological progress of modern qualitative
identification technology has been very much, but limited, especially to identify unknown
materials. Because if you use identification technology with modern and sophisticated
tools, it will cost a lot and takes a long time.
We realized that this guidebook is far from perfect and will develop with the
development of new drugs. We request for advice and criticism in the perfection of this
teaching material. Hopefully this textbook will benefit all of us. Thank you.
Medan, Februari 2020
Author.
Do not copy or reproduce the contents of this book
without the written permission of the author
3
CONTENTS
Preface
Contents
Experimental techniques in qualitative analysis
Percobaan 1 Dry Analysis (uji nyala, sublimasi, pirolisa)
Percobaan 2 Analysis of Cation (Ag+,Pb+2,Hg+2,Bi+3,Cd+2,Cu+2,As+3,Fe+2,Fe+3)
Percobaan 3 Analysis of Cation (Al+3, Zn+2, Ca+2, Ba+2, Mg+2,K+, Na+, NH4+)
Percobaan 4 Analysis of Anion (Cl-, Br-, I-, NO2-, NO3
-, PO43- ClO-)
Percobaan 5 Analysis of Anion (SO42-,SO3
2-,S2O32-, CO3
-2, HCO3-,borat, tetraborat)
Percobaan 6 Practical Test of Cation and Anion
Percobaan 7 Functional Group dan Infra red Analysis
Percobaan 8 C,H,O Compound Analysis
Percobaan 9 C,H,O,N Compound Analysis Part I
Percobaan 10 C,H,O,N Compound Analysis Part II
Percobaan 11 C,H,O,N,S Compound Analysis
Percobaan 12 Practical Test
4
Experiment 1
Dry Analysis
Aim:
In order for students to carry out cation and anion tests, sublimation tests and pyrolysis
crystals which can be used in the preliminary test analysis of certain compounds.
DRY ANALYSIS AND CRSYTAL REACTION
include: flame test with Ni / Cr wire, Cu wire, sublimation, pyrolysis and crystal reaction.
1. Flame test with Ni/Cr wire.
Objective: to know the specific flame colour of several cations.
How: Ni / Cr wire is cleaned by dipping the wire into concentrated HCl (in a tube
or watch glass), then burned. Performed repeatedly until the flame of the Bunsen
on the combustion wire did not provide a special flame colour. Then the wire is
moistened with concentrated HCl and dipped in the sample, so that there is a little
sample attached to the end of the wire, then burned again, observe the flame
colour.
The experiment was repeated for another sample after the wire was cleaned.
Compare the results with the theory you know.
Sample : K+, Ba+2, Ca+2, As+3, Na+ .
Compound Flame colour
K
As
Ba
Ca
Na
Purple
Grey
Greenish yellow
Red
Golden Yellow
5
2. Flame tests with Cu wire ( beilstein Test).
Objective: to know the flame colour of halogen / halogenide.
The ways: copper wire is cleaned by rubbing it using sand paper, then burned.
Performed repeatedly until the flame of the Bunsen on the combustion wire did
not provide a special flame colour. Dip the end of the wire in a sample / sample
solution, burn and observe the flame colour.
The experiment was repeated for another sample after the wire was cleaned.
Sample: Cl-, Br-, I-.
3. Pyrolysis Test.
Objectives: 1. To find out whether there is residual pyrolysis or not, if the
inorganic compound is burned.
2. To see the specific colour of the remaining pyrolysis of some
metal oxides.
The ways: provide a clean porcelain cup / crucible. Place a small amount of solid
sample in the saucer, heat it over the fire, first with low heat, observe and note the
color changes that occur. Then the fire is raised and burning continues until there
is no change/ there is no black color on the cup. Record the color of the remaining
pyrolysis for each sample.
Sample : NH4Cl, ZnO, Pb(CH3OO)2, Bi(NO3)3, Hg(NO3)2.
4. Sublimation Test.
Objective: to find compounds that are easily sublime.
The ways : provide a sublimation ring and a clean glass objects. Place a small
amount of solid sample into the sublimation ring that has been placed above the
glass object, then close the ring with a glass object again and above it is given
cotton that has been dripped with water. Then heated with a low heat. Look the
shape under a microscope and draw it.
Sample: H3BO3, As2O3.
6
5. Crystal reaction from Cations :
Zn with K2Hg(CNS)4
Ca with oxalic acid
K with picric acid
Na with picric acid
7
Experiment 2
Analysis of Cation
Aim:
In order for students to analyze the cations contained in a sample.
Cations Identification : Ag+, Pb+2, Hg+2, Bi+3, Cd+2, Cu+2, As+3, Fe+2, Fe+3
Students are given 1 sample that contain one of the above cations.
Stages Analysis:
1. Organoleptic Tests: Smell, Colour and Taste
2. Flame Test with Ni / Cr
3. Classification Test
a) Group 1 cation deposition reaction
b) Group 2 cation deposition reaction
4. Specific reactions
Perform a minimum specific test if the sample is suspected
Sample: Ag+
• with dilute HCl
percipitate + dilute NH4OH
Dilute HNO3
• percipitate + water, heat it up ,observe after cold
• with KI
percipitate + concentrated NH4OH
percipitate + KCN,
• with K2CrO4
• with sulfide solution
• with α.α'dipiridil
• with Ditizon
8
Sample: Pb2+
• with dilute HCl
percipitate + dilute NH4OH
percipitate + water, heat it up
observe after cold
• with KI
percipitate + water, heat it up
percipitate + excessive KI
• with K2CrO4
• with sulfide solution.
• with dithizon reagents
Sample : Hg2+
• with sulfide solution (HCl acid atmosphere)
+ excessive sulfide solution
• with NaOH
+ NaOH excess
• with KI
+ KI excess
• with Difenyl Carbazid
• with Dithizon
Sample: Bi3+
With sulfide solution
o + HCl dilute
with KI
o + KI excess
with Na2HPO4
with Pirogallol and HNO3 dilute
with dithizon
9
Sample : Cd2+
sulfide solution
With NH4OH
o + NH4OH excess
With KCN
With Difenylcarbazid
Sample : Cu2+
with sulfide solution
o percipitate + HNO3 heat it up
with NH4OH
o percipitate + NH4OH excess
with K4[Fe(CN)6]
with KCN
with KI
with dithizon
Sample : As3+
with Sulfide solution + HCl dilute
Gutzeit test.
With AgNO3
o Percipitate + HNO3
With sol. Iodii
Sample : Fe2+
Sulfide solution
with K3[Fe(CN)6]
with α α’ dipiridil
with dimetilglioksim
with o-fenantrolin
10
Sample : Fe3+
with NaOH
o + NaOH excess
Sulfide solution
With K4[Fe(CN)6]
with NH4CNS
11
Experiment 3
Analysis of Cation
Aim:
So that students can analyze the cations contained in a sample
Identification of cations: Al+3, Zn+2, Ca+2, Ba+2, Mg+2,K+, Na+, NH4+
Practically given 1 sample containing one of the above cations
Stages of analysis:
1. Organoleptic Test: Odor, Color and Taste
2. Flame Test with Ni / Cr
3. Classification Test
a. Group III cation deposition reactions
b. Group IV cation deposition reactions
c. Group V cation
4. Specific reactions
Perform a minimum specific test if the sample is suspected
Sample: Al3
• with NaOH
o + NaOH excess
• with sulfide solution
• with Alizarin
• with Aluminon
• with dithizon
Sample: Zn2+
• with NaOH
12
o + NaOH excess
• with sulfide solution
• with Na2HPO4
• with dithizon
• reaction of crystals with KHgCNS (crystal image
Sample: Ba2 +
• with (NH4) 2CO3
o sediment + HNO3 e
• with H2SO4 e (crystal image)
• with K2CrO4
• with meditren solution
Sample: Ca2 +
• with H2SO4 (crystal image)
• with (NH4)2(COO)2 (crystal image)
• with K4[Fe(CN)6]
• with Meditren (crystal image)
Sample: Mg2 +
• with NH4OH e
o sediment + NH4Cl
• with (Na) 2CO3
o sediment + NH4Cl
• with Na2HPO4 +
o NH4Cl + NH4OH
• with Titan Yellow
o + NaOH
Sample: K +
• with Na Cobaltritrite
• with tartric acid (crystal image)
13
• with perchloric acid (crystal image)
• with picric acid (crystal image)
Sample: Na +
• with Zink uranyl acetate (crystal image)
• with picric acid (crystal image)
Sample: NH4 +
• with NaOH
o test with litmus
o test with a stirring rod dripped with HCl
• with Nessler
• with Na.cobaltinitrit
• with Tanin and AgNO3 solutions
14
Experiment 4
Analysis of Anion
Aim:
So that students can analyze the anions contained in a sample.
Anion identification: Cl-, Br-, I-, NO2-, NO3
-, PO43-, ClO-
Practically given 1 sample containing one of the anions above.
Stages of analysis:
1. Organoleptic Test: Odor, Color and Taste
2. Flame Test with Cu
3. Classification Test
a. Anion reaction with acid addition
b. The deposition reaction with silver nitrate, barium clorida, magnesium
sulfate and other salts
c. Oxidizing properties test
d. Reducing properties test
4. Specific reactions
Perform a minimum specific test if the sample is suspected
Sample: Cl-
• with AgNO3
o sediment + NH4OH e
o solution + HNO3 e
• with Pb.acetat
o sediment + water, heat after cold observe
• with KMnO4 + H2SO4
• test with Kanji / KI paper
15
Sample: Br-
• with AgNO3
o sediment + NH4OH e
o sediment + NH4OH p
• with Pb.acetat
o sediment + water, heat, observe after cold
• with NaOCl + HCl,
o shake with CHCl3
• with KMnO4 + H2SO4
o test with starch paper
• with K2Cr2O7 + H2SO4
Samples: I-
• with AgNO3
o sediment + NH4OH e
o sediment + NH4OH p
• with Pb.acetat
o sediment + water, heat observe after cold
• with NaOCl + HCl e
o shake with CHCl3
• with KCr2O7 + H2SO4
o test with starch paper
Sample: NO2-
• with KMnO4 / H2SO4
• KI solution
• with FeSO4 / H2SO4
• with Antipirin and HCl
16
Samples: NO.3-
• with H2SO4 p
• with FeSO4 / H2SO4 p
• reduction with Zn / HCl
o + antipyrin and HCl
• with diphenylamine / H2SO4
• with Zn / NaOH
o test with tanin solution and AgNO3
Sample: PO43-
• with AgNO3
o sediment + NH4OH e
o sediment + HNO3 e
• with FeCl3
o sediment + CH3COOH
o sediment + HNO3
• with HNO3
• with BaCl2
o sediment + HCl e
Sample: OCl-
• KI + H + → I2 solution
o I2 release test
• with HCl e
o test with starch paper
• with Pb. acetat
17
Experiment 5
Analysis of Anions
Aim:
To allow students to analyze anions are present in a sample.
Identification anion: SO42-, SO3
2-, S2O32-, CO3
-2 , HCO3-, BO3
3-, B4O72-
Students are given one sample that you lack any of the above anions.
Stages of analysis:
1. Test organoleptic: Odor, Color and Flavor
2. Test Bright with Cu
3. Classification Test
a. The reaction by the addition of acid anion
b. Precipitation reaction with silver nitrate, barium chloride, magnesium
sulphate and other salts
c. Tests oxidant properties
d. Reductant nature test
4. Specific reaction
Make a minimum specific test if the sample allegation
Sample: SO42-
with BaCl2
o sediment + HCl e
o sediment + HNO3 e
with Hg(NO3)2
with Pb.acetat
Sample: SO32-
HCl e
o test with K2Cr2O7
18
o KIO3 starch test paper
with KMnO4 + H2SO4
by the K2Cr2O7 + H2SO4
with a solution of Fuchsin
Sample: S2O32-
with a solution Iodii
with AgNO3
with Pb.Acetat
o preheat the sludge + water
with NaOH + KCN, heat + HCl + FeCl3
Sample: CO32-
HCl e
o test with stir bar that drops of Ba(OH) 2
with BaCl2
o sediment + HCl e
with AgNO3
o sediment + NHOH
o sediment + HNO3 e
with MgSO4
o heat
with HgCl2
with CaCl2
o sediment + NH4OH
o sediment + HCl e
Sample: CO32-
the sample was heated
o test with whitewash
with MgSO4
19
o heat
HCl e
o test with Ba(OH)2
with CaCl2
o sediment + NH4OH
o sediment + HCl e
with HgCl2
o sediment + HCl e
with AgNO3
o sediment + NH4OH
o sediment + HNO3 e
Sample: BO33-
sublimation test
o crystal image
borax esterification with CH3OH and H2SO4p
o heat
with phenolphthalein and 1 or 2 drops of NaOH to react weakly
o + 1 drops of glycerin,
Sample: B4O72-
Borax esterification with CH3OH and H2SO4p
o heat
with AgNO3
o sediment + NH4OH
o sediment + CH3COOH
o heated deposition
with BaCl2 dropwise until excess
with phenolphthalein
o + 1 drops of glycerin
20
Experiment 6
Practical Test of Cation and Anion
Aim:
To allow students to analyze cations and anions are present in a sample.
Identification Cation and Anion (from experiments 2-5)
Students are given one sample containing cations and anions
Stages of analysis:
1. Test organoleptic: Odor, Color and Flavor
2. Test Bright with Ni / Cr
3. Test Bright with Cu wire
4. Classification Test
a. Cation precipitation reaction group 1
b. Cation precipitation reaction group 2
c. Cation precipitation reaction group 3
d. Group 4 cation precipitation reaction
e. Reaction cation identification group 5
f. Identification reaction with concentrated acid anion
g. Anion precipitation reaction with silver salts, magnesium, zinc and barium
h. The oxidation reaction anion
i. The reduction reaction anion
5. Specific reaction
For specific reaction clay at 2-5 experiments.
21
Experiment 7
Functional Groups and Infrared Analysis
Aim:
- So that students can analyze functional groups contained in a sample using chemical
reactions.
- So that students can analyze functional groups contained in a sample using infrared
spectrophotometry method.
Cation identification: Function group
Practicum is given 1 sample containing organic compounds to be analyzed for its
functional groups.
1. Aliphatic hydroxy group
Mono Hydroxy Aliphatic
• Azo's reaction
• Esterification reactions
Poly Hydroxy Aliphatic
• Azo's reaction
• Test with Borat / can increase the acidity of Borat solution.
• Cuprifill reactions
2. Hydroxy aromatic group
Mono Hydroxy Aromatic
• Azo's reaction
• Reaction of FeCl3
• The reaction of the Marquis
Poly Hydroxy Aromatic
• Azo's reaction
• Reduction Reactions to Fehling and Ammonia Silver
22
3. Carboxyl group
• Test for positive carbonyl
• Esterification reactions
4. Keton group
• Reaction with Na. Nitroprussid (Rothera Legal Reaction)
• Iodoform reaction
5. Aldehyde group
• Schiff's reaction
• Reduction of Tollen’s reagent and Fehling
6. Amin group
• Reactions with p-DAB HCl
• Reactions with matchstick
• Indophenol reaction
• Reactions with CuSO4
7. Nitro group
• Reactions with bases of NaOH or KOH
• Reduction in acidic conditions to primary amine.
8. Sulfon group
• Oxidized to SO42-, and identified as SO42-
9. Unsaturated bond
• The reaction is added to Aqua Brom
• Reaction to KMnO4 solution (Baeyer reaction).
23
Cation identification: Function group
Practitioner is given 3 samples containing organic compounds to analyze the functional
group content using a spectrophotometer. Students interpret spectrum data obtained.
Tools and materials:
• IR plate
• Mortar and pestle
• Cotton bud
• Tissue
• KBr for IR
• Acetone
• Sample
Procedure:
Prepare samples to be examined. The sample must be pure compound. If in solid form it
must be the result of crystallization or the results of isolation by chromatography. The
liquid sample is purified by distillation or gas chromatography.
Samples are mixed in special mortar and pestle with paste-forming compounds (Nujol,
hexachlorobutadiene, fluorolube) or pellets. The most commonly used pellet is KBr,
because it does not provide specific absorption. Before measuring sample absorption,
measurements of absorption from the pasta or pellet maker were measured. The aim is to
reduce the absorption caused by the humidity of the environment against the absorption
of samples obtained.
Comparison of mixing samples with KBr or Nujol is 1 mg: 100 mg, or it can be said to be
1% sample. The maximum measurement sample that still gives good results is with a
sample content of 10%.
24
INTERPRETATION OF INFRARED SPECTRUMS
-COOH 3600 – 2400 cm-1
-OH 3500 – 3200 cm-1
-NH2 3500 – 3100 cm-1
=C-H 3150 – 3050 cm-1
-C-H (alifatis) 2950 – 2875 cm-1
-COH (aldehid) 2750 cm-1
CΞC 2250 – 2100 cm-1
CΞN 2250 cm-1
C=O 1700 cm-1
C=C 1600 and 1500 cm-1
N=O 1550 – 1350 cm-1
S=O 1350 – 1050 cm-1
C-O 1300 – 1000 cm-1
CH2 1450 cm-1
CH3 1375 cm-1
C-C 1200 cm-1
C-Cl 800 cm-1
C-Br 550 cm-1
C-I 500 cm-1
25
Experiment 8
Analysis of Compounds C, H, O
Aim :
In order for students to be able to carry out identification reactions of compounds that
have elements C, H and O with functional groups OH Aliphatic and Aromatic both
monovalent and polyvalent, and carboxylic groups and able to distinguish compounds
from one another (especially those used/ related to the pharmaceutical field), by using
certain chemical reagents.
Compounds carried out by practicum include:
1. Organic compounds used in the pharmaceutical field which have elements C, H, and O
with OH Aliphatic functional groups in the form of monovalent or polyvalent.
2. Organic compounds used in the pharmaceutical field which have elements C, H, and O
with OH functional groups in the form of monovalent or polyvalent
3. Organic compounds used in the pharmaceutical field that have C, H, and O elements
with the -COOH functional groups in the form of mono carboxylic and poly
carboxylic.
General reaction to OH aromatic:
1. AZO Reagent Reaction:
Diazo A: 0.5% sulfanylic acid solution in (30 ml 4N HCl + 70 ml water).
Diazo B: 9% NaNO2 solution in water.
How to experiment:
Add 2 drops of ethanol or a sample solution in water into the test tube, add Diazo A
and Diazo B (4: 1 or 1: 1) and 1-2 drops of NaN 2N until reacting alkaline, shake, heat
it in a water bath, it will form a color reddish yellow to red. Add 4 drops of amyl
Functions C, H and O Aliphatic, shake, color not interested Amyl Clusters of C, H and
O Aliphatic functions. (colorless layer). (for groups of function groups C, H and O
Aliphatic).
26
Try the same for glycerin, observe and record the results.
Compare the results that occur in all samples examined.
2. Esterification reaction. (Monovalent Aliphatic)
Reactor :
Salicylic acid, benzoic acid or acetic acid.
Concentrated sulfuric acid as a catalyst.
How to experiment:
3 drops of ethanol are put into the test tube, add a little salicylic acid crystals and 1-2
drops of concentrated H2SO4, cover the mouth of the tube with wet cotton, heat it in a
water bath for 5 minutes. Lift and dilute with 1 ml of water. Smell the smell and smell
of gandapura (for ethanol and methanol).
The experiment was repeated using benzoic acid or acetic acid. Observe and note the
smell.
3. Reaction of the committee. (Aliphatic polyvalent)
Reactor :
2% CuSO4 solution, 2N NaOH solution
How to experiment:
Add a little glycerin (or sample solution in water) into the test tube, add 1 solution of
CuSO4 and 2-3 drops of NaOH solution, clear blue dark solution will form. Heat,
don't form red brick deposits.
Perform the same experiment on ethanol, observe and record the results.
Compare the results that occur in all samples examined.
4. Test with Borax. (Aliphatic polyvalent)
Reactor :
1% borax solution and 0.2% phenolphthalein solution in 70% ethanol.
How to experiment:
In the test tube put 1 drop of borax solution and 1 drop of phenolphthalein solution
(the solution becomes red). Add 2 drops of glycerin. Observe and record the results.
Do the same experiment with ethanol, observe and record the results; compare results
in all samples.
27
5. Carletty's reaction. (Aliphatic polyvalent)
Reactor :
Oxalic acid (crystal)
Resorcin (crystal)
Concentrated H2SO4
How to experiment:
2 drops of glycerin free of water (or a small amount of solid sample) is placed on the
drip plate, add a little bit of oxalic acid crystals and a bit of resorsing crystals, stir with
the stirring rod, then add 1 drop of concentrated H2SO4, stir, observe and record the
results.
Perform the same experiment on ethanol, observe and record the results. Compare
results for all samples.
General reaction to the Aromatic OH group:
1. Azo reaction (same as in C, H and O Aliphatic functional groups, but red can form
in cold conditions, if shaken with amyl alcohol, generally red can be attracted to
amyl alcohol). (for OH Aromatic groups).
2. Reaction with FeCl3
On the drip plate, a small sample or solution of neutral sample in water or ethanol is
added 1 drop of FeCl3 solution, color will be formed depending on the sample
being examined. (observe the color changes that occur).
3. Reaction with aqua bromine
In a test tube (or drip plate) place a small amount of the sample solution (in water
or ethanol), add aqua brom drop by drop, (observe the results of the reaction on the
addition of a little aqua bromine, and on adding aqua bromine).
4. Lieberman's reaction (reaction with concentrated NaNO2 and H2SO4).
Reagent: 1% NaNO2 solution in concentrated H2SO4 (made new)
How to: put a little sample or sample solution into the test tube, add 1-2 drops of
reagent, leave a few minutes, then dilute with a few drops of water, will form a red
color, mix with NaOH or NH4OH, the color turns blue.
28
5. The reaction of the Marquis:
Reagent: mix 1 part formaldehyde with 9 parts H2SO4 solid (made new).
Method: on a drip plate a small amount of solid sample is added with 1 drop of
reagent, a color will be formed.
6. Reactions with Fehling reagents (for polyvalent phenols).
In the test tube enter 2-3 drops of the sample solution in water, add 2 drops of
fehling A and 2 drops of fehling B, if necessary heat it in the water, it will form a
yellow to brick red precipitate.
7. Reactions with silver ammonia (for polyvalent phenols)
Reagent: 0.5 ml AgNO3 0.1N added dilute ammonia drop by drop until the
precipitate formed dissolves again.
How to: a few drops of sample in the tube are added a few drops of reagent, if
necessary, heat the water bath, a silver mirror is formed on the tube wall.
8. The reaction with floroglusin and NH4OH or NaOH (for polyvalent OH
Aromatic), fluoroglusin reagent and NaOH 0.5 N or concentrated NH4OH.
Method: 1 drop of sample solution + a little fluoroglusin crystal + a few drops of
water + 1 drop of NaOH, stir the color.
or concentrated NH4OH, stir the color.
Based on the results of the reaction above a special reaction is carried out on OH
aromatic which is examined or suspected, according to each monograph.
General properties of carboxylic acid compounds:
Generally acidic, can react with bases to form salts that are easily soluble in
water.
Dignified acid 1 which has a short C chain, in the form of a liquid that is easy to
mix / dissolve in water. The longer the C chain, the harder it is to dissolve in water.
Aromatic acid is generally difficult to dissolve in water.
Many dignified acids are generally easily soluble in water.
29
Identification of carboxylic acid compounds.
Given the absence of a general reaction to carboxylic acids, the identification
reaction is carried out on functional groups which may be present in the carboxylic
compounds examined.
Stages of Analysis:
1. Organoleptic test (shape, smell, taste and color)
2. Test solubility (in water or in organic solvents), then apply it over a water bath.
3. Beilstein and Ni/ Cr flame tests
4. Fluorescence
5. Pyrolysis
6. Azo's reaction
7. Esterification reaction
8. The reaction of Cuprifil
9. Carletty's reaction
10. Borax reactions
11. Iodoform reaction
12. Fehling's reaction
13. Silver Ammonia Reaction
Subsequent examinations were carried out based on the results obtained in the
above test, in accordance with the monograph of each suspected C, H and O Clusters.
Examples of several Pharmaceutical compounds that have elements C, H and O with
OH functional groups are Aliphatic and Aromatic:
1. METHANOL (CH3OH)
2. ETHANOL (C2H5OH)
3. CHLORAL HYDRATE (CCl3-CH (OH) 2.)
4. GLYCEROL (Glycerin = propane triol: CH2 (OH) -CH (OH) -CH2OH)
5. GLICOL ETILEN. (HOCH2-CH2OH)
6. PROPILEN GLICOL (Trimethylene glycol: CH3-CHOH-CH2OH)
7. MANNITOL
8. SORBITOL
9. PHENOL
30
10. NIPAGIN (Methyl p hydroxy benzoate) preservative
11. NIPASOL (Propyl p hydroxy benzoate) Preservatives
12. VIOFORM (Iodochloro hydroxy quinoline) Antiamuba
13. RESORSINOL (m-dioxy benzolum) Keratolytic
14. HIDROQUINON. (p-dioxy benzolum)
15. DERMATOL (Bismuth sub gallat) Antiseptic
16. GUAIPHENESIN (GLYCERIL GUAIACOL) Expectorant
17. ACETIC ACID (Vinegar acid: CH3 - COOH)
18. ACID BENZOAT
19. SODIUM BENZOAT
20. SALICYLATE ACID
21. SODIUM SALISILATE
22. ACID ACETYL SALISILATE
23. CITRIC ACID
24. SRIUM SITRAT
25. TARTRATE ACID
26. POTATO HYDRAULIC TARTRATE (Cream of tartar).
27. VITAMIN C (ASCORBIC ACID)
31
Experiments 9 and 10
Analysis of Compound C, H, O and N (I and II)
Aim :
1. So that students are able to perform the reactions to identify pharmaceutical
compounds containing elements C, H, O and N, by the reaction classification and
the functional group contained in each compound.
2. So that students are able to distinguish the pharmaceutical compounds containing
elements C, H, O and N with each other based on reactions that occur.
Nearly 75% of pharmaceutical compounds containing the element nitrogen compounds
derived from both natural and synthetic made paracetamol Nitogen in pharmaceutical
compounds are usually bound in the form of: a bond with the nitro compounds into
carbon compounds, as amine primary, secondary or tetsier alkaline; as ammonium
kiuarterner; aromatic amine groups, acid amide neutral zwitterion salts such as amino
acids. Compounds that have the elements C, H <O and N contained in compounds that
have pharmacological effects such as barbital, Vitamins, Antibiotics and Anti-histamine
in addition to compounds derived from nature such as alkaloids and amino acids
Public reaction
1. As Aromatic Nitro.
The principle of this method changes aromatic nitro into primary aromatic
amines.
How it works: A number of 50 mg of aromatic nitro compounds dissolved in
ethanol add 3 ml of dilute HCl, 4 ml of water and 200 mg Zn, in the water bath
heated mixture of water for 10 minutes, then add 2 drops of reagent A. Further
Diazo solution is poured into 2 ml Diazo reagent B; formed orange or orange
precipitate Example: nitrazepam.
2. Aliphatic primary amine
Reaction Sentol: Addition to Carbon Disulfides
32
How it works: A solution aliphatic amine compounds dissolved in ethanol and
then sprinkled with carbon disulfide as much, is heated to evaporate the excess
CS2, the rest of adding HgCl2 solution, showed a distinctive smell of the aliphatic
primary amine Example; Amitriptyline, Cinnarizine, Ethambutol, Methadone,
Pethidine, Propranolol, Timolol and Verapamil.
3. Basa Compound Amine
Reaction Mayer; Amine base compound forms a precipitate yellowish.
How it works: basic amine compounds dissolved in the water, if insoluble added
sulfuric acid and hydrochloric acid in order to form a clear solution, and then
inserted into the test tube was added some drops of reagent Mayer then
precipitates yellowish. The reaction can also be done in the object glas. Chinin
example HCl, Coffein.
4. Aromatic Primary Amines
Diazo reaction
Ways of working ; Number 50 mg primary aromatic amine compounds dissolved
in 1 ml of HCl 3N, the solution was treated with 2 drops of Diazo A Furthermore,
the solution is poured into 2 ml of reagent Diazo B; orange or red color formed
orange precipitate positive reaction to benzocaine, Procaine and the reaction is
positive when first added in the water bath HCl and heated water for 10 minutes
prior written Diazo Diazo A and B, Klordiazopoxid example, HCT, Oksazepam
and phenacetin.
5. Secondary Amines
Flourescamine test
How it works: Compounds of amine secondary dissolved in 2 ml of HCl 3 N
cooled to 5 ° C and then added 2 ml solution of NaNO2 1%, allowed to stand for
5 minutes, then the solution is diluted with water 5 ml and shaken twice, each
shuffling added ether 5 ml, grab ether and washed and evaporated to dryness, the
rest of the evaporation was added phenol 50 mg, briefly heated, cooled and
treated with 1 ml of H2SO4 formed in red and ar formed when diluted with red
color.
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6. The imidazole compound
The reaction with sulfanilic acid terdiazotasi
How it works: nitrogen compounds having a group of imidazole dissolved in 3 N
NaOH 1 ml and then added a solution of sulfanilic acid (0.5 grams of sulfanilic
acid dissolved in 70 ml of water and then reacted with HCl 6 N 6 ml add water to
100 ml ) and 10% NaOH at a lot of it will form a red color Example: Paracetamol
For nitrogen compounds can also be done the following general reaction:
1 reaction Dragendorf
2 reaction Bauchardat
3 Ninhydrin reaction
4 Ortho degan reaction Phtalaldehyde / Betta- Mercaptoetanol.
5 reaction Isonitriles
6 Condensation with 1,2 naphthoquinone Sodium 4 sulfonate
7 Reaction with nitric acid.
Stages Analysis:
1. Test organoleptic (shape, smell, taste and color)
2. Test solubility (in water or in organic solvents), then uapkan over a water bath.
3. Test flame Beilstein and Ni / Cr
4. fluorescence
5. pyrolysis
6. Public reaction
Examples of Pharmaceutical Compounds That Has Some Elements C, H, O and N
1. GLUTAMIC ACID (HOOC-CH (NH) 2- (CH2) 2-COOH)
2. MEFENAMIC ACID
3. NICOTINE ACID
4. NICOTINAMIDE
5. P-AMINO SALICYLIC ACID
6. INH, ISONIAZID
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7. DIPHENHYDRAMIN HCl
8. ANTIMO
9. EPHEDRINE
10. SALBUTAMOL
11. BENZOCAIN
12. PROCAIN HCl
13. LIDOCAIN HCl
14. PARACETAMOL
15. PHENACETIN
16. ANTIPIRIN
17. PHENYL BUTAZONE
18. CAFFEINE
19. THEOHYLLINE
20. TEOBROMIN
21. QUININE
22. QUININE HCl
23. QUININE Sulfat
24. PAPAVERIN HCl
25. KODEIN HCl
26. DEXTROMETHROPHAN HBr
27. NOSCAPIN
28. CHLORAMPHENICOL
29. CHLORAMPHENICOL Palmitat
30. CHLORAMPHENICOL Stearat
31. PHENOBARBIT
32. DIPHENILHIDANTOIN
33. STREPTOMISIN
34. TETRACYCLIN HCl
35. OKSITETRASIKLIN HCl
36. CHLOR PHENIRAMIN MALEAT
37. ANTAZOLIN HCl
35
38. VITAMIN B6
39. VITAMIN M
40. VITAMIN B2
36
Experiment 11
Analysis of Compound C, H, ON and S
Aim :
So that students are able to perform the reactions to identify pharmaceutical
compounds containing elements C, H, O, N and S, based on the reaction classification
and the functional group contained in each compound.
Sulfur element of the analysis:
1. With the method lassaigne
2. Reduction with a strong reducing agent
Compounds containing elements of S can be divided into several Alignment:
1. Thiols and disulfan
2. Tio ether compound
3. sulfone compound
4. Sulfonic acid derivatives
5. Sulfonyl urea compound
6. heterocyclic compounds
Stages Analysis:
1. Test organoleptic (shape, smell, taste and color)
2. Test solubility (in water or in organic solvents), then apply it over a water bath
3. Test flame Beilstein and Ni/ Cr
4. fluorescence
5. pyrolysis
6. Public reaction
37
Examples of Pharmaceutical Compounds That Has Some elements C, H, O, N and S
1. AMPISILLIN
2. AMOKSISILLIN
3. ANTALGIN
4. SULFACETAMID
5. SULFADIMIDIN
6. SULFADIAZIN
7. SULFAGUANIDIN
8. SULFAMERAZIN
9. SULFASOMIDIN
10. SULFANILAMID
11. SULFATIAZOL
12. SULFAMETOXAZOL
13. CHLORPROMAZIN HCl
14. PROMETHAZIN HCl
15. MEBHIDROLIN NAPADISYLATE
16. THIAMIN HCL (Vitamin B1)
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Experiment 12
Practical Test
Aim :
So that students are able to carry out reactions to identify pharmaceutical
compunds containing compounds of all elements namely C, H, O, N, and S based on
functional groups and classification analysis found in each compound.
Analysis Step:
1. Organoleptic Test (shape, smell, taste and color)
2. Solubility test (in water or organic solvent), then evaporated over the bath
3. Flame Test Beilstein and Ni/Cr
4. Fluorescence
5. Pyrolisis
6. General Reaction
7. Special reaction/ specific
The sample tested was one of all samples analyzed from experiment 8 to 11.
39
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