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.

33

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

34

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)

38

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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