1 TECHNICAL REPORT ON STUDENT INDUSTRIAL WORK EXPERIENCE SCHEME (S.I.W.E.S) AT NATIONAL AGENCY FOR FOOD AND DRUG ADMINISTRATION AND CONTROL (NAFDAC) CENTRAL DRUG QUALITY CONTROL LABORATORY,8/10 MERRIT ROAD, YABA, LAGOS STATE. BY JAMES DAVID OMEIZA MATRIC NUMBER: 100804045 THE DEPARTMENT OFCHEMISTRY FACULTY OF SCIENCE UNIVERSITY OF LAGOS,AKOKA,YABA FROM MAY-OCTOBER,2013 IN PARTIAL FULFILMENT OF THE REQUIREMENT FOR THE AWARD OF BACHELOR OF SCIENCE (B.Sc.)
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1
TECHNICAL REPORT
ON
STUDENT INDUSTRIAL WORK EXPERIENCE SCHEME
(S.I.W.E.S)
AT
NATIONAL AGENCY FOR FOOD AND DRUG ADMINISTRATION AND CONTROL (NAFDAC) CENTRAL DRUG QUALITY CONTROL LABORATORY,8/10 MERRIT ROAD, YABA, LAGOS STATE.
BY
JAMES DAVID OMEIZA
MATRIC NUMBER: 100804045
THE DEPARTMENT OFCHEMISTRY
FACULTY OF SCIENCE
UNIVERSITY OF LAGOS,AKOKA,YABA
FROM
MAY-OCTOBER,2013
IN PARTIAL FULFILMENT OF THE REQUIREMENT FOR
THE AWARD OF BACHELOR OF SCIENCE (B.Sc.)
2
ACKNOWLEDGEMENTS
All glory and honour to God Almighty for the grace he has given me to take part in the industrial training programme. To my wonderful guardians, pastor and pastor Mrs Johnson for
their everlasting support, prayers and all round encouragement throughout the training period.
I also want to say a big thank you to my parents, Mr and Mrs James for their kind words and
encouragement, my lecturers,my Institution based supervisor Dr (Mrs) Tolu Fashina, course
adviser, Dr (Mrs) Rose Alani, my Industry supervisor Mr Adeyemo Idowu for his fatherly love, ,
fellow I.T students and all the staffs of NAFDAC who has contributed in one way or the other to
the success of this report.
3
DEDICATION
This report is dedicated to my heavenly Father for strength and provision to continue throughout
the period of the Industrial training and the will never to give up in life and also to my guardians
for their parental love and support.
4
CERTIFICATION
This is to certify that this report is put together by James David Omeiza, a student of the
department of chemistry,University of Lagos on completion of the Student’s Industry Work
Experience Scheme.
________________________ ______________________
STUDENT SIGNATURE INSTITUTION-BASED
SUPERVISOR
5
ABSTRACT
This report is a summary of all the work experience I have been able to gather during my SIWES
training programme at National Agency for Food and Drug Administrations and Control
(NAFDAC).
The report contains some of the tests that are carried out on drug samples by NAFDAC to
ensure that they are safe for the consumption of Nigerians.
The report is separated into chapters with each chapter from chapters 4 to chapter 8 stating
everything I have learnt in each laboratory for simplicity reasons.
This report also containwhat I is taught by the various analysts I worked with and informations
I got from text books, online during my SIWES training in the agency.
This report is restricted to drugs and chemicals.The procedures for the various tests conducted
on drug samples are shown. Calculations whose results help the analysts to determine whether
a drug sample is passing or failing are also shown.
In conclusion, this technical report is the summary of what I have learnt during my Industrial
training programme.
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TABLE OF CONTENTS Pages
Title page 1
Acknowledgement 2
Dedication 3
Certification 4
Abstract 5
Content 6
Chapter 1.0Introduction 7-11
Chapter 2.0History of agency (NAFDAC) 12-15
2.1 Evolution of regulatory activities 2.2 Brief History of NAFDAC 2.3 Mission of NAFDAC 2.4 Mandate of NAFDAC 2.5 Agency chart of the agency
Chapter 3.0My Work Experience 16
Chapter 4.0 Cosmetics Laboratory 17-22
Chapter 5.0 Pharmacognosy Laboratory 23-32
Chapter 6.0 High Performance Liquid Chromatography 33-38
Chapter 7.0 Pharmaceutical Control Laboratory 39-46
Chapter 8.0 Conclusion and recommendations, summary and reference. 47-48
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CHAPTER ONE
INTRODUCTION
The Students’ Industrial Work Experience Scheme (SIWES) wasstarted in 1974 by Industrial
Training Fund (ITF) with about 748 students from 11 institutions of higher learning. This
became very necessary when it is discovered that theoretical knowledge alone would not usually
prepare an educated person for the world of work. Therefore the need to set up a scheme to train
students ( particularly for those pursuing careers in sciences, engineering and technology
disciplines SET ) not only to be knowledgeable in their fields but to be able to apply the
acquired knowledge and skills to perform defined jobs or work. There is a demand for a new
cadre of workers having a range of skills across related disciplines and not theoretical experts in
a single discipline. Such a wide range of skills, as being demanded by the world of works today,
cannot be readily acquired through theoretical training alone but in combination with training.By
1978, the scope participation in the scheme had increased to about 5,000 students from 32
institutions.
The Students’ Industrial Work Experience Scheme (SIWES) is a Skill Training Programme
designed to prepare and expose students of the University to the industrial work situation they
are likely to meet after graduation. The need for the establishment of the scheme arose when
there is a growing concern among industrialists that graduates of institutions of higher learning
lacked adequate practical background required for employment in industries.
The Students Industrial Work Experience Scheme has contributed immensely to the building the
common pool of technical and allied skills available to the Nigerian economy which are needed
for the nation’s industrial development. These contributions and achievements have been
possible because of regular innovations and improvement in the modalities employed for the
management of the scheme. SIWES forms part of approved minimum academic standard in the
various degree programmes for all the Nigerian Universities. It serves as an effort to bridge the
gap existing between theoretical knowledge Obtained during lectures with the actual industrial
conditions.
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OBJECTIVES OF THE STUDENTS’ INDUSTRIAL EXPERIENCE SCHEME (SIWES)
Theoretical Knowledge alone would not usually prepare an educated person for the world of
work. The worker or productive individual must not only be knowledgeable but must also be
versatile in the application of skills to perform defined jobs or work.
SIWES is an integral part of most degree and diploma programmes in institutions of higher
learning in Nigeria. The scheme is designed to take place in institutions outside the schools and it
has a realistic relevance to development of manpower in Nigeria.
The reality of the programme can be illustrated using a simple analogy. While it is possible for
someone to learn and imbibe all the available information on driving a car in the classroom, it is
unlikely that the individual would, based on the knowledge alone, be able to drive a car at the
first opportunity. On the other hand, someone else without the theoretical information on how to
drive a car, on being told and shown what to do, followed by hands-on practice and supervision
by an instructor, would at the day be able to drive a car successfully. Of course, someone who
has been exposed to both theoretical underpinnings of driving a car and the hands-on experience
of doing so would and should be a better driver.
Consequently, there are two basic forms of learning – education and training – both of which are
indispensable to the production world of work and the functioning of the society at large. In the
illustration given above, the first individual had abundant education on how to drive a car; the
second individual had adequate training on how to drive a car; the third individual had the
advantage of being able to combine theoretical knowledge with practical skills to become a
better driver.
Some other reasons why the training is indispensable in the formation of competent and
productive SET graduates include those mentioned below
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TRAINING IN THE FORMATION OF SET GRADUATES
Scientists, engineer and technologists cannot be produced purely by education. They need
practical training to equip them with the tools of their trade in order to enable them make
contributions to industrial development. It is impossible for a fresh SET graduate from a
university or polytechnic to be competent to carry out the functions of his or her chosen field
effectively. The knowledge in one’s head does not translate directly into goods and services. It is
though the intermediation of practical application that theoretical knowledge becomes
productive. While institutions of learning provide the basic education, competence in carrying
out tasks, jobs, work and functions is acquired through training in the work place. Industrial
training, therefore, provides the avenue for undergraduates to acquire the basic tools of their
future professions while still being students.
1.3 EXPECTATIONS AND PERCEPTIONS OF EMPLOYERS
Gap between the learning acquired by graduates of Nigeria’s tertiary institutions, particularly
SET graduates and the skills repertoire required in the workplace. Employers believe that Nigeria
graduates bring sufficient theoretical knowledge to the job but that they generally lack hands-on
or practical skills and orientation that would make them productive. Industrial training provide a
veritable means of addressing and redressing the gaps between the skills repertoire possessed by
students and the relevant production skills (RPSs) required by employers.
1.4 RELEVANCE OF SIWES
One of the significant features of advanced industrial societies is the degree to which they have
achieved progress in the field of science and technology. This had enabled the citizens to enjoy a
good standard of living, which exceeds that of the developing Countries. Thus, formal education
comprising of field or industrial work is vital for the production of graduates with increasingly
specialized skill.
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Therefore, Students Industrial Work Experience Scheme (SIWES) is relevant for;
Improvement of science and technological education
Skilled manpower development
Creation of a community with increased standard of living
Development of critical and scientific approach to problems and their solutions.
New innovations in the field of science and technology.
As a matter of fact, the student’s industrial work Experience scheme (SIWES) is a promotion for
the growth of science and technology, Engineering, Agriculture, Medical, Management, and
other professional programmes in the Nigerian tertiary Institutions.
1.5 BENEFITS OF INDUSTRIAL TRAINING TO STUDENTS
The major benefits accruing to students who participate conscientiously in industrial training are
the skills and competencies they acquire. These relevant production skills (RPSs) remain a part
of the recipients of industrial training as lifelong assets which cannot be taken away from them.
This is because the knowledge and skills acquired through training are internalised and become
relevant when required to perform jobs or functions.
Several other benefits can accrue to students who participate in industrial training. These include
the following:
Opportunity for students to blend theoretical knowledge acquired in the classroom with
practical hands-on application of knowledge required to perform work in industry.
Exposure of students to the environment in which they will eventually work, thereby
enabling them to see how their future professions are organized in practice.
Minimization of the bewilderment experienced by students, particularly those from non-
technological background, pursuing course in science, engineering and technology with
regard to different equipment, processes, tools etc, available in industry.
Enabling SET students appreciate work methods and gain experience in handling
equipment and machinery which may not be available in their institutions
11
Preparing students to contribute to the productivity of their employers and national
development immediately after graduation.
Provision of an enabling environment where students can develop and enhance personal
attributes such as critical thinking, creativity, initiative, resourcefulness, leadership, time,
management, presentational skill, interpersonal skills, amongst others.
Preparing students for employment and making the transition from school to the world of
work easier after graduation.
Enhancing students’ contacts with potential employers while on training.
Enabling students bridge the gap between the knowledge acquired in institutions and the
relevant production skills (RPSs) required in work organizations.
Making SET students appreciate the role of their professions as the creators of change
and wealth and indispensable contributors to growing the economy and national
development.
Enabling students appreciate the connection between their courses of study and other
related disciplines in the production of goods and services.
1.6 PLACE OF TRAINING
I was privileged to have my industrial training at National Agency For Food And Drug
Administration And Control. I was posted to four different Laboratories in the agency where I
worked.The report is based on what I have learnt so far in the agency.
My first training in the agency is safety precautions and good manufacturing practice of the
agency.
GOOD MANUFACTURING PRACTICE (GMP); There are different categories of GMP.
Hygiene for personnel on arrival at work:
clean hair, hands, nails and body
Nails to be clipped short
Leave personal items in your locker
Wash and sanitize hands
Wearing of safety goggle within the laboratory department.
Wearing of gas mask when dealing with chlorine gas
Wearing of safety boot within the laboratory department of the agency.
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CHAPTER TWO
EVOLUTION OF REGULATORY ACTIVITIES
In 1970, there is no specified body charged with the responsibility of ensuring that food and drug
product meets the international standard.
During these periods, between 1930 and 1976, the federal government performed this function
until the food and drug administration and laboratory services (FDALS) took over.
Existing legislative provision for the control of the quality and safety of food and drug decree in
1974,fake and substandard drug decree No.41 of 1990 and the National Agency For Food and
Drug Administration and Control (NAFDAC) decree No. 15 of 1993 of all these, the latest
regulatory body is NAFDAC, which is regulated by the food and Agricultural Organization
(FAO)
A BRIEF HISTORY OF NAFDAC
The organization is formed to checkmate illicit and counterfeit products in Nigeria in 1993 under
the country’s health and safety law.
In one 1989 incident, over 150 children died as a result of paracetamol syrup containing
diethylene glycol. Such problem lead to the establishment of NAFDAC, with the goak of
eliminating counterfeit pharmaceuticals, food and beverage products that are not manufactured in
Nigeria and to ensure that available medications are safe and effective.
In December 1992, NAFDAC’s first governing council is formed. The council is chaired by
Ambassador Tanimu Saulawa. In January 1993, supporting legislation is approved as legislative
decree No. 15 of 1993. On January 1, 1994, NAFDAC is officially established as a “parastatal of
Federal Ministry of Health”. NAFDAC replaced an earlier Federal Ministry of Health body, the
directorate of Food and Drug Administration and Control, which has been deemed ineffective,
partially because of lack of laws concerning fake drugs.
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MISSION OF NAFDAC
The mission of National Agency for Food and Drugs Administration and Control is to
Create more laboratories for easier accessibility which are being equipped to function
effectively.
Organize more workshops to enlighten various stakeholders such as pure water
producers, Patent and Proprietary Medicine Dealers Association (PPMDA), National
Union of Roads and Transport Workers (NUIRTW) etc.
Continue to raise awareness not just in Nigeria but also in other countries like India,
China, Pakistan and Egypt
Hold meetings with chairman, House Committee on Health and its members with
Ambassadors of countries identified with exporting fake drugs into Nigeria and solicit
their support to stop the trend
Achieve excellent results in the fight against counterfeit drugs, as evidenced by the public
destruction of about 2 billion Naira worth of drugs from four sources, namely those
handed over by the repentant traders, those found in secret warehouses on tip off by the
drug sellers and the public and those seized by the drug sellers’ internal task forces and
NAFDAC task forces.
Hold consultations with national and international stakeholders leading to various areas
of assistance, including areas of staff training, equipment donations and information
sharing from United States Food and Drug Agency (USFDA), World Health
Organization (WHO), International Narcotics Control Board (INCB),Environmental and
Occupational Health Science Institute (EOHSI), putting new guidelines and standard
operating procedures (SOP) in place for all regulatory processes
MANDATES OF NAFDAC
The National Agency for Food and Drug Administration and Control has three major mandates
which are:
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1. Timely
2. Quality
3. Standard
This means that analytical results should be produced on time and the result produced must be of
good quality to meet international standards.
NAFDAC has various basic functions. According to the requirements of its enabling decree, the
Agency is authorized to:
Regulate and control the importation, exportation, manufacture, advertisement,
distribution, sale and use of drugs, cosmetics, medical devices, bottled water and
chemicals
Conduct appropriate tests and ensure compliance with standard specifications designated
and approved by the council for the effective control of quality of food, drugs, cosmetics,
medical devices, bottled water, and chemicals.
Undertake appropriate investigation into the production premises and raw materials for
food, drugs, cosmetics, medical devices, bottled water and chemicals and establish a
relevant quality assurance system, including certification of the production sites and of
the regulated products
Undertake inspection of imported foods, drugs, cosmetics, medical devices, bottled
water, and chemicals and establish a relevant quality assurance system, including
certification of the production sites and of the regulated products.
Compile standard specifications, regulations, and guidelines for the production,
importation, exportation, sale and distribution of food, drugs, cosmetics, medical devices,
bottled water, and chemicals
Undertake the registration of food, drugs, medical devices, bottled water and chemicals
Control the exportation and issue quality certification of food, drugs, medical devices,
bottled water and chemicals intended for export
Establish and maintain relevant laboratories or other institutions in strategic areas of
Nigeria as may be necessary for the performance of its functions.
Issuing quality certification of food, drugs, cosmetics, medical devices, bottled water and
chemicals intended for exports.
Undertake measures to ensure that the use of narcotic drugs and psychotic substances are
limited to medical and scientific purposes
Collaborate with the National Drug Law Enforcement Agency in measures to eradicate
drug abuse in Nigeria.
Finally amongst others, NAFDAC has been mandated to enforce the decree No. 15 of
1993 and impose sanctions on violators of these decrees and regulation under it. All the
above mentioned mandates of NAFDAC involving the functional role of a food ,
laboratory scientist, and technologist who tries to work alongside other agencies.
15
NAFDAC ensures it maintains very close contact with a number of national and international
organizations whose activities relate to the functions of NAFDAC. Such organizations include
the following
Consumer Protection Council of Nigeria (CPC)
The National Drug Law Enforcement Agency (NDLEA)
The for Pharmaceutical Research and Development (NIPRD)
The Pharmacist Council of Nigeria (PCN)
The Federal Environmental Protection Agency (FEPA)
Institute of Public Analyst of Nigeria
Association of Beverages and Tobacco Employees of Nigeria
Association of Nigeria Custom Licensed Agents (ANCLA)
AGENCY CHART OF NAFDAC (Central Drug Quality Control Laboratory) Yaba.
CHAPTER THREE
16
CHAAPTER THREE
MY WORK EXPERIENCE
During the period of my Industrial training in NAFDAC,I is posted to the following laboratories:
1. Cosmetics Laboratory (Lab 6)
2. Analytical Chemistry Laboratory (Lab 2)
3. Pharmacognosy Laboratory (Lab 7)
4. High Performance Liquid Chromatography Laboratory (Lab 1)
5. Research and Validation Laboratory (Lab 9)
6. Pharm Control Laboratory (Lab 3)
Other functional laboratories within the agency include :
1. Micro Drug Laboratory (Lab 11)
2. Pharmacology Laboratory (Lab 8)
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CHAPTER FOUR
4.0 COSMETICS LABORATORY
This Laboratory deals with the analysis of cosmetics products and veterinary drugs (Animal
drugs). These products are analysed to know if they are safe for human use or animal
consumption. The kind of test(s) to be carried out on these products depend on the type of
product to be analysed. Examples of cosmetics products analysed in the laboratory and the
parameters tested on them include:
Soaps : Net weight, total fatty matter, free caustic alkali, chloride content, moisture
content, pH, hydroquinone and mercuric compound.
Shampoo: Filling volume, pH, Non-volatile matter and Chloride content.
Toothpaste: Net weight, pH, Total solid matter, fluoride content.
Perfume : Filling volume, pH, Specific gravity, volatile matter, Zirconium.
Powder: Net weight, moisture content, bulk density.
Relaxer : Net weight, pH, NaOH content, CaOH content and non-volatile matter
Detergent: Net weight, moisture content, pH, Chloride content, Total active matter.
The various tests carried out on cosmetic samples can be divided into two.They are Identification
tests and physical parameterstests.
4.1 Identification Tests: These tests are carried out on samples to know whether the
compounds used in manufacturing the products as claimed by the manufacturers are present or
not and also to know if the product contains any harmful compound such as mercuric compound
or hydroquinone that is harmful to the consumer.Some of these compounds used in the
manufacturing of cosmetics products include : NaOH, CaOH, Chlorides, Vitamin E, Lanolin,
glycerinetc. For both NaOH and CaOH. Titration is used to quantify the amount present.
4.1.1Physical Parameters Tests : These tests are used to measure the filling volume of liquid
samples, net weight of solid samples, texture,. moisture content, pH (10%),bulk density etc.
18
4.2 PROCEDURES ON HOW TO PERFORM SOME OF THE PHYSICAL
PARAMETERS TESTS CARRIED OUT ON COSMETICS SAMPLES
4.2.1 Net Weight
This test is done on solid, powdered or detergent samples such as soaps, creams, toothpastes etc
to know if the actual weight claimed by the manufacturer is true. The analytical weighing
balance is used for this purpose.
Apparatus - Weighing boat, spatula
Instrument – Analytical weighing balance
Procedure : The sample and the weighing boat is weighed together at first to obtain the total
weight. The content of the weighing boat is then emptied and the empty weighing boat weighed
to obtain the empty weight. The empty weight subtracted from the total weight gives the net
weight. This is then divided by the claimed weight and then multiplied by 100 to obtain the
percentage weight.
Total weight – Empty weight = Net weight.
Actual weightx100
Claimed weight 1
Note : The percentage net weight of the sample must not be less than 95% for the sample to pass
the test.
4.2.2 Filling Volume
This analysis is carried out on liquid samples such as shampoo, syrup, perfume etc.
Apparatus – Measuring cylinder
Procedure : The content of the sample Is emptied into a measuring cylinder
and the volume is read on the calibration along the side of the measuring cylinder.
19
% Filling volume = Filling volume × 100
Claimed volume
4.2.3 pH (10%) Test
pH is a measure of the amount of hydrogen ion concentration present in a solution. In other
words, it is the negative logarithm of the hydrogen ion concentration. The pH level of a sample
gives us an idea of the level of the acidity or alkalinity of the sample. Acidity increases as pH
value decreases and alkalinity increases as pH value increases. This test is carried out on any
sample in liquid form or the solution of the sample (if it is in solid or powdery form) in order to
determine if the sample is acidic, basic or neutral. The range of pH within which a sample must
fall into in order to pass the pH test varies from one sample to another. For example here is a
table showing some of the samples and their PH ranges.
1.Soaps/detergents/relaxers 9.5 – 12.0
2. Powder 7.0 – 9.5
3. Perfume/antiperspirant/shampoo/creams 4.0 – 7.5
4. Jelly/pomade Neutral
5. Hair conditioner/activator/gel 3 - 8
Apparatus – 10ml measuring cylinder, beaker
Instruments – Water bath, pH meter
Aim – To determine the pH value of a sample
Procedure: For liquid samples such as methylated spirit, about 10 ml of the sample is measured
into a clean 25 ml beaker or for solid or semi-solid samples such as a toilet soap,1g of it is
weighed into a clean 25 ml beaker, then 10ml of distilled water (PH 10 %) is added and warmed
slightly to dissolve in a water bath. This is then allowed to cool and then taken to the PH meter to
take the PH reading by Inserting the electrode of the PH meter into the sample in the beaker, the
read button ispressed on the PH meter and allowed to read until a square root sign appears on the
20
reading (which indicates the final stable reading).Then the reading isrecorded including the
temperature on the screen
Diagram of a pH meter Water Bath
4.2.4 Moisture Content:
This is done on cosmetic samples using the moisture analyzer machine to determine the amount
of the sample that will evaporate. The result obtained here is displayed in percentage and is
referred to as the Volatile matter of 1gram of the sample while the result subtracted from 100 is
the Non-Volatile matter.
Apparatus – Evaporating pan, spatula
Instrument – Moisture analyzer
Aim – To determine the amount of volatile matter present in a cosmetic sample.
Procedure:1g of a detergent is placed In an evaporating pan and the machine is operated. When
the the machine finish analysing the sample,a beeping sound is made by the machine which
indicates the end of the process and the value on the screen is recorded as the Volatile matter
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MOISTURE ANALYZER
4.3 PROCEDURES ON HOW TO PERFORM IDENTIFICATION TESTS FOR COSMETICS
PRODUCTS
Apparatus – Test tubes, spatula, beakers, 10ml measuring cylinder
Reagents – 2 M Sodium Hydroxide, ethanol, 10% potassium iodide, Iodine solution, conc
H2SO4, Chloroform, distilled water
Hydroquinone : Hydroquinone is a bleaching agent and is tested for in creams and
soaps.
According to the agency, the concentration of Hydroquinone should not be more than 2% if
present in cosmetics products because it causes skin rashes.
Procedure: To 2 ml of the sample solution, about 1-2 drops of 2 M Sodium Hydroxideis added.
Brownish color develops which intensifies with more drops of Sodium Hydroxide indicated its
presence.
Mercuric compound : Mercury is a cancer causing agent and should not be present in
cosmetics products at all.
22
Procedure: To the sample solution, ethanol and 10% w/v potassium Iodide solutionis carefully
added. A red precipitate is formed which is soluble in excess reagent if present.
Alcohol: This test is carried out on samples to confirm the presence of alcohol in any
product that has alcohol as one of the active ingredients as claimed by the manufacturer.
Procedure: To 5 ml of the sample solution,1 M NaOHis first added, then 2 ml of I2 solutionis
added, Iodoform developed and yellow precipitate isformed.
Note:If yellow color isnot formed, add acidified Potassium dichromate solution. This turns to
green on warming.
Reaction 1 - Oxidation of ethanol by NaOl ( compound formed by the reaction between I2 and
NaOH ).
Reaction 2 & 3 - Substitution of Hydrogen by I2 in the presence of OH-.
Reaction 4 – Breaking of c-c bond by OH-
This reaction is known as Iodoform reaction.
Lanolin: This should not be present especially in baby cosmetic products because it can
cause red or swollen skin and itching.
Procedure:50 mg of sampleis dissolved in 5 ml of Chloroform.5 ml of concentrated H2SO4is
added to it and shaken. Red color developed and appearance of green florescence on the upper
layer is observed which indicated the presence of lanolin.
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5.0 CHAPTER FIVE
PHARMACOGNOSY LABORATORY (LAB 7)
This is the laboratory where herbal and non-herbal drugs are analysed. The drugs can either be in
tablets, capsules, syrups or as a tea in tea bags. The following are the tests carried out on herbal
and non-herbal drugs:
1. Identification test for phytochemical parameters (for herbal drugs only)
2. Drug Compliance Number test (DCN)
3. Drug Registration Number test (DRN)
5.1 IDENTIFICATION TEST FOR PHYTOCHEMICAL PARAMETERS
This test is carried out on herbal drugs to identify the presence of phytochemical
parameters/ingredients in them. These phytochemical compounds include : flavone, caffein,
saponin, alkaloid, glycoside, tannin etc.
The reagents used for these tests are Meyers reagent, distilled water, 10% NaOH, 10 % Ethanolic
KOH ,2 M HCl and 1% Ferric Chloride. These tests are carried out in a fume cupboard using test
tubes,beakers and spatula. The table below shows the reagents used, the test, observation and
results obtained when these tests/analysis were carried out on herbal drug sample.
PARAMETER TEST OBSERVATION INFERENCES
1. Glycoside About 100mg of the
sample is placed in a
test tube,10ml of
ethanolic KOH is
added to it and shaken
If pink / red coloration
is observed
Glycoside is present
2. Tanin To about 100 mg of
the analyte in a test
tube isadded 1%
Ferric Chloride and
If blue/green
coloration is observed
Tanin is present
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the solution shaken
3. Saponin To 100mg of the
sample isadded 5ml of
distilled water and
shaken
If foaming or frothing
is observed
Saponin is present
4. Alkaloid 5ml of Meyer’s
reagent is added to
100mg of the sample
If pale brown color is
formed
Alkaloid is present
5.Flavone To about 100mg of
the analyte,5ml of
10% NaOH is added
and shaken
If yellow coloration is
formed
Flavone is present
Test for Total Chloride Content
We test for the total chloride present in oral dehydration drugs and quantify the amount present
through titration with AgNO3. Usually we have 2 types of Chloride present in Oral Dehydration
salts which are NaCl and KCl
Apparatus : beakers, conical flasks , burette
Reagents : 0.1 M AgNO3, dilute HNO3, Distilled water
Procedure:
Fill the clean dry burrette with 0.1M AgNO3. Weigh about 1g of the salt into a dry conical flask,
add 30ml of distilled water followed by a few drops of dilute HNO3.Titrate the solution in the
conical flask against the 0.1M AgNO3. If Chloride ion is present, white precipitate is formed.
NaCl + AgNO3 →NaNO3 + AgCl
25
Example
Actual Yield
Gross weight = 28.6859g
Empty weight = 1.3470g
Net weight = 28.6859 – 1.3470
= 27.3389g
Total Chloride Content
Weight taken = 1.0193g
Titre Value = 31ml
Constant = 0.003545
Concentration = 31 × 0.003545
= 0.109895
If 1.0193g of salt contains 0.109895 chloride,
27.3389 = 27.3389 × 0.109895
1.0193
Total Chloride present = 2.9475212
Theoretical Yield
NaCl = 35.5 × 3.5
58.44
= 2.126112
KCl = 35.5 × 1.5
74.55
= 0.7142858
NaCl + KCl = 2.126112 + 0.7142858
Theoretical yield = 2.8403979
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% Claim = 2.9475212 × 100
2.8403979
= 103.77%
The % claim is within 90% - 110%. Therefore the salt passed the test.
Test for Glucose content
The glucose content of a salt is usually tested for by following the procedure below
Procedure
Apparatus : 100ml volumetric flask, cork, spatula
Reagents : Concentrated Ammonia, distilled water.
Instrument : Photometer
Determine the net weight of the salt (same as above). Weigh about 2g of the salt into a 100ml
volumetric flask. Add 60ml of distilled water. Then add 5 drops of concentrated Ammonia. Cork
the flask and allow to stand for 1hour. Then make it up to the 100ml mark with water and
proceed to the photometer to take 3 absorbances.
Example
Net weight = 27.3389g
Weight taken = 2.0216g
Absorbance measured = 1.65, 1.66, 1.63
Δf (Dilution factor) = 100 = 1
100
Constant = 0.9477
Concentration = Optical reading × constant × Δf × Net weight
Net weight
27
= 1.63 × 0.9477 × 1 × 27.3389
2.0216
Concentration = 20.890281g
Claim = 20g
%Claim = 20.890281g× 100
20g
%Claim = 104.45%
Since the %Claim falls within 90%-110%, the salt passed the Glucose test.
5.2 DRUG COMPLIANCE NUMBER ANALYSIS
This test is also known as determination of physical parameters of a sample. Under this test,
description of the physical properties of the sample (such as shape, color, texture, viscosity,and
uniformity of weight etc). The test is carried out on tablets, capsules, syrups, injections and
suspensions. The agency performs this test on new drugs whose manufacturers have applied for
NAFDAC registration number newly to know if such drug complies with the acceptable
standards of the British Pharmacopia (B.P) or United States Pharmacopia (U.S.P).The test is also
performed on drugs that already has NAFDAC registration number if new batches of such drugs
are produced in order to check if the new batch still complies with the U.S.P/B.P standards as the
previous batch. If the drug fails the DCN analysis, it means there is something wrong with the
physical parameter(s) of the drug depending on which parameter it fails. The applicant is notified
in this case and asked to reanalyse their drugs before bringing it back for analysis by the agency.
But if it passes, DRN test is then carried out on them.
5.2.1 METHOD OF ANALYSIS FOR DRUG COMPLIANCE NUMBER (DCN)
TABLETS AND CAPLETS
- 20 tablets of the sample is placed in a weighing boat
28
- All the 20 tablets is weighed using an analytical weighing balance to obtain the total
weight of 20 tablets
- Then the individual weights of the 20 tablets is also obtained.
- The average weight of the tablet is calculated using the formular below
Average weight = Total weight of 20 tables
Total number of tablets weighed
- The percentage deviation is calculated using the table and the formular below
% Deviation = k x Average weight
100
AVERAGE WEIGHT OF TABLETS DEVIATION (k)
1. 80 mg or less 10.0
2. > 80 mg but < 250 mg 7.5
3. 250 mg or more 5.0
- The uniformity of weight is then calculated using the formular below
Upper Limit (U.L) = Average weight + % Deviation
Lower Limit (L.L) = Average weight – % Deviation
The uniformity of weight is said to be satisfactory if all the individual weights of the 20
tablets/caplets fall within the upper and the lower limit. Hence the sample has passed DCN test.
FOR CAPSULES (Hard gelatin or soft gelatin)
- 20 capsules is placed in a weighing boat
- The total weight of the 20 capsules is taken to obtain the total gross weight
- The individual weight of each of the 20 capsules is also obtained and the empty weights
of each of them
- The empty weights subtracted from the gross weights of the individual capsules gave
their net weights
- Then the empty weights of all the 20 capsules is weighted In order obtain total empty
weight
29
- The total empty weight of all the 20 capsules subtracted from the total gross weight gave
the total net weigh
- The total net weight is divided by the number of capsules (20 capsules) to obtain the
average weight of a capsule.
- Then the % deviation calculated using the table and the formular below
% Deviation = k × Average weight
100
Upper Limit = Average weight + % Deviation
Lower Limit = Average weight – % Deviation
AVERAGE WEIGHT OF CAPSULES DEVIATION (k)
1. < 300 mg 10.0
2. 300 mg or more 7.5
Example: To carry out DCN analysis on Metformin Hydrochloride tablet
Procedure:
Total weight of 20 tablets = 15.2282g
Average weight of 20 tablets = 15.2282g ÷ 20
= 0.76141g
Individual weights
1. 0.7654g 6. 0.7720g 11. 0.7623g 16. 0.7427g
2. 0.7442g 7. 0.7828g 12. 0.7494g 17. 0.7837g
3. 0.7671g 8. 0.7794g 13. 0.7718g 18. 0.7724g
4. 0.7486g9. 0.7461g 14. 0.7380g 19. 0.7656g
5. 0.7606g 10. 0.7562g 15. 0.7479g 20. 0.7586g
30
Average weight = 15.2282g ÷ 20
= 0.76141 g
Deviation (k) from the table for tablets above = 5
% Deviation = 5 × 0.76141
100
= 0.0380705
Upper Limit (U.L) = 0.76141g + 0.0380705
= 0.7994805g
Lower Limit (L.L) = 0.76141g – 0.0380705
= 0.7233395g
Since all the individual weights fall within the upper and lower limits, uniformity of weight is
satisfactory and hence the sample has passed the DCN test.
FOR SUSPENSIONS, INJECTIONS AND SYRUPS
SUSPENSION
- The suspension is first Reconstituted with equivalent liquid such as distilled water to the
mark on the container
- The fill volumeis determinedwith a measuring cylinder
- The pH of the suspension is taken using the pH meter
- The weight per ml is also estimated.
To do this, the analytical weighing balance is switched on and zeroed. Then the weight of a
5ml volumetric flask is taken. The volumetric flask is filled to the mark with the reconstituted
suspension and the total weight is taken. Then the weight of 5ml of the suspension is
obtained by subtracting the initial weight from the final weight.The result is then divided by
5 to obtain the weight per ml.
31
INJECTIONS
- Determine the fill volume by using a syring
- Determine the pH
- Determine the weight per ml
SYRUPS
- Determine the fill volume by using a measuring cylinder
Calculate the % fill volume using
%Fill volume = Fill volume / claimed fill volume× 100
- Determine the weight per 5ml
- Determine the pH value using the pH meter
5.3 METHOD OF ANALYSIS FOR DRUG REGISTRATION NUMBER (DRN)
DRN test is carried out on drug samples that do not have NAFDAC registration number. It is
usually referred to as an ASSAY. Assay is an investigative procedure in the laboratory analysis
for quantitatively measuring the presence or amount of a target entity. The measured entity is
generally called the analyte (Wikipedia).
After the physical parameters test (DCN) is carried out on the drug sample, the said drug must
pass the DRN test in addition to the DCN test before the issuance of NAFDAC registration
number.
The aim of this analysis is to quantify the amount of the active pharmaceutical ingredient present
in the drug sample. The method of analysis used by the analyst in analysing these drugs is
usually reviewed from the Standard Operating Procedure (S.O.P). The S.O.P is gotten from
either U.S.P or B.P which are standard compendia for the preparation and analysis of drugs. The
acceptable limit for Active Ingredient that must be present in the drug sample is between 90%
and 110%.
32
5.3.1 PROCEDURE FOR DRUG REGISTRATION NUMBER ANALYSIS (ASSAY)
Carry out DCN test on the drug sample in order to obtain the average weight of the drug (
for tablets, capsules or caplets) or determine the weight per ml of the drug sample if it is
in liquid form (in case of injections, suspensions and syrups)
Check the S.O.P for the method of analysis of the particular active ingredient being
worked on.
Prepare the solution of the drug sample following the method of analysis stated in the
S.O.P (which should contain the Molar Absorptivity E1)
Find the weight taken by using the formular
Weight taken = Average weight (g) × equivalent (mg)
Claim (mg)
Calculate the dilution factor using the formula
Dilution factor = a / 100 × b/c × d/e…….
Where a = First volume make up
b = Second volume make up
c = No of mls taken from first volume make up
d = No of mls taken from second volume make up
e = Third volume make up
Shake or sonicate the final solution if stated in the S.O.P
Proceed to the UV-Visible Spectrophotometer . Blank machine with the solvent used to
prepare the solution of the sample. Then take at least 4 absorbances of the prepared
solution of the drug sample.
Finally calculate the % active ingredient as shown below using Beer-Lambert’s law
which states that “a decrease in the intensity of a monochromatic radiation is proportional
to the amount or concentration of absorbing specie in its path and the intensity of the
incident radiation. This law relates the absorption of light to the properties of the
absorbing specie/material through which the light is passing. Mathematically
where A= absorbance
33
E= Molar absorptivity (L mol-1cm-1
)
l=Path length of cuvette (1cm)
C= Concentration (L mol-1)
i. Concentration = Absorbance × Dilution factor
Molar Absorptivity (E1)
ii. Active Ingredient (AI) = Average weight(mg) × concentration × 1000
Weight taken(mg)
iii.% Active ingredient (%AI) = AI (gotten from step ii)(mg) × 100
Actual Claim (mg)
EXAMPLE OF DRN TEST OR ASSAY
Standard Operating Procedure for Metformin Hydrochloride
The method of analysis stated in the S.O.P for the analysis of Metformin Hydrochloride
says: Weigh and powder 20 tablets. Take an equivalence of 100 mg Metformin
Hydrochloride from the powdered tablets into a 100ml volumetric flask. Add 70ml of
distilled water to it and shake for 15 minutes (At 100 rpm).Then dilute further with
distilled water and make it up to the 100ml mark. Filter the solution (discarding the first
20ml).Take 10ml of the filtrate into another 100ml flask, make up to the mark.Then
finally dilute 10ml of the resulting solution into another 100ml flask and make up to mark
with distilled water. Measure the absorbance of the resulting solution @ 232nm, E1=798.
Procedure:
Apparatus – weighing boats, spatula, 4 100ml volumetric flasks, plastic corks, 2 beakers,
3 1.5mm filter papers, funnel
Reagents – Distilled water
Instruments – Analytical weighing balance, UV-Visible Spectrometer, cuvette
Average weight = 0.76141g
34
Claim = 500mg
Weight equivalent = 100mg
Equivalent weight = 0.76141g × 100mg
500mg
Equivalent weight = 0.152282g
Then a weight very close to 0.152282g
Weight taken = 0.1533g
Dilution factor = 100 × 100 × 100
100 10 10
Dilution factor = 100
Absorbance @232 = 0.74756, 0.74470, 0.74302, 0.74627
Note: None of the absorbance taken must be less than 0.2 and none must be greater than
0.8. Meanwhile the absorbance values must be close to each other i.e precise
Concentration = Absorbance × Dilution factor
E1
= 0.74756g × 100
798
Concentration = 0.0936792g
Active Ingredient = Concentration × average weight (g) × 1000g
Weight taken(g)
AI = 0.0936792 × 0.76141g × 1000mg
0.1533g
AI = 465.29mg
% Active Ingredient = 465.29mg × 100
500mg
%AI = 93.057%
35
Hence the sample passed the Assay.
NB: The standard acceptable pass limit is between 90% - 110%. If the %AI obtained is greater
than 110%, it means that the active ingredient is in excess therefore the drug is considered not
safe for human consumption. If the active content is lower than 90%, the drug has also failed as
it will be ineffective when taken by the consumer.
These are some of the instruments used in the laboratory for analysis
Analytical weighing balance UV-Visible spectrometer
Shaker Fume cupboard
36
6.0 CHAPTER SIX
6.1 HIGH PERFORMANCE LIQUID CHROMATOGRAPHY LAB
High Performance Liquid Chromatography Lab of the agency is the analytical chemistry
laboratory that uses the HPLC machine to carry out analysis on drug samples with two or more
active pharmaceutical ingredients. The HPLC instrument operatesby using a separation
technique known as chromatography.
Chromatography is a separation technique that relies on the different abilities of substances to
adsorb or stick to surfaces. The mixture to be separated is dissolved in a fluid or an unreactive
gas such as helium or nitrogen known as the mobile phase which carries it through a structure
holding another material called the stationary phase. The various constituents of the mixture
travel at different speeds along the stationary phase causing them to separate.
Liquid chromatography can be divided into normal phase or reverse-phase chromatography
depending on which is more polar between the stationary phase and the mobile phase
Normal Phase Liquid Chromatography (NPLC) - This technique uses columns packed
with polar stationary phases (hydrophilic) combined with non-polar or moderately polar
mobile phase (hydrophobic) to separate the components of a mixture. The hydrophilic
stationary phase has high affinity for hydrophilic molecules in the mobile phase. The rate
at which the individual solutes migrate through the columns is primarily a function of
their polarity. Less polar solutes move the fastest and therefore exit the column and are
detected first, followed by solutes of increasing polarity which move more slowly.
Reverse Phase Liquid Chromatography (RPLC) – Reverse Phase Liquid
Chromatography is just the opposite of Normal Phase Liquid Chromatography in that it
uses a non-polar stationary phase (hydrophobic) while the mobile phase is polar
(hydrophilic). The HPLC instrument
uses the reverse phase liquid chromatography technique. An inert non-polar substance
that achieves sufficient packing is used in Reverse phase liquid chromatography as the
stationary phase column. According to what I is told and shown by one of the analysts in
the agency, the HPLC machine uses octadecyl carbon chain (C18) or octyl carbon chain
(C8) as its stationary phase column. There are other columns like phenyl bonded silica.
37
The mobile phase used to elute analytes from the reverse phase column is usually a
mixture of water or aqueous buffers and organic solvents. The solvents used must be
miscible with water. Examples of such solvents are acetonitrile and methanol.
The agency makes use of High Performance Liquid Chromatography (HPLC) machine which is
an improved form of Liquid chromatography and employs the reverse phase technique in its
operation. The HPLC machine is an instrument used for analysing drug samples with more than
one active ingredient or multivitamins because such drugs are always difficult to analyse with a
U-V spectrometer.High Performance Liquid Chromatography (HPLC) is a separation technique
that involves the injection of a small volume of liquid sample or the solution of a sample into a
tube packed with tiny particles called the stationary phase where individual components of the
sample are moved through the packed tube (stationary phase) with a liquid (mobile phase) forced
through the stationary phase by high pressure delivered by a pump. These components are
separated from one another by the stationary phase (packed tube) using the various physical and
chemical interactions between their molecules and the packing particles in the tube. These
separated components are detected at the exit of the packed tube by a detector that measures the
amount of each component present. An output from this detector is called a chromatogram.
Diagram of a labelled modern HPLC machine
Injector
Column (stationary
phase) and column
oven
Pump
Detector
Data acquisition,
control and
display unit
Mobile phase and
mobile phase reservoir
38
6.2PARTS OF AN HPLC MACHINE
The High Performance Liquid Chromatography is made up of sixmain parts which are:
1) Mobile phase and mobile phase reservoir:Mobile phase helps to transport the sample
through the column and it must be such that it does not react with the sample it is
transporting. Pure solvents or buffer combinations are commonly used. The mobile phase
should be free of particulate impurities. Mobile phase reservoirs are inert transparent
weighing boats for storing and holding the mobile phases in place for easy transport.
Generally, transparent bottles are used to facilitate visual inspection of mobile phase level
inside the weighing boat. Particulate filters are also provided inside the weighing boat to
remove impurities from the mobile phase if there is any present.
2) Pumps: Variations in flow rate of the mobile phase affects the elution time of an analyte
which usually results in errors . Therefore a pump provides constant flow of the mobile
phase to the column (stationary phase) at a specific flow rate expressed in milliliters per
minute ml/min. A pump can deliver a constant mobile phase composition (isocratic) or an
increasing mobile phase composition (gradient). Normal flow rates in HPLC are in the
range of 1-2 ml/min and can reach a pressures in the range of 400-600 bar.
3) Injectors: Injectors are used to provide constant volume injection of samples into the
mobile phase stream. There are two types of injectors and they are manual injector
(where the analyst injects the sample into the stream using manual process) and Auto-
sampler (which automatically injects a specific/constant volume of the sample into the
mobile phase stream). Inertness and reproducibility of injectors are necessary to maintain
high level of accuracy. The injector must also be able to withstand the high pressures of
the pump
4) Column (stationary phase): This is where the separation of the sample components take
place using various physical and chemical parameters. A column is a stainless steel tube
packed with the stationary phase.It is a vital component of the HPLC machine that must
be maintained properly in order to get reproducible separation efficiency run after run.
5) Column Oven: Variation in temperature during the analytical run can result in changes of
retention time of the separated eluting components. A column oven maintains a constant
39
column temperature using air circulation. This ensures constant flow of mobile phase
through the column.
6) Detector: Detector gives specific response for the component separated by the column
and also provides the required sensitivity. The detector detects the individual molecules
that are eluted from the column and measures the amount of those molecules so that the
chemist can quantitatively analyze the sample components by providing an output to a
computer which is displayed as a graph called the chromatogram. Majority of the
applications require UV-VIS detection though detections based on other detection
techniques are also available.
7) Data Acquisition, control and Display Unit (The computer system): Modern HPLC
machines are computer based and software controls parameters such as temperature, flow
rate, injection volume, sequence and also acquisition and treatment of output. The
computer not only controls all the modules of the HPLC instrument but it takes the signal
from the detector and uses it to determine the time of elution (Retention time) of the
sample component (qualitative analysis) and the amount of the sample component
present (quantitative analysis).
6.3OPERATION OF THE HPLC MACHINE
In the laboratory, I.T students are not allowed to operate the HPLC machine but can help in the
preparation of mobile phases (buffers or solvents), samples containing the active ingredients and
reference standards.
At the beginning of an analysis, the mobile phase flows steadily and continuously from the
mobile phase reservoir which is usually placed on top of the machine into the pump. The pump
then exerts reasonable amount of pressure on the mobile phase that will be enough to pass it
through the column. The reference standard active pharmaceutical ingredient and the sample
containing the active ingredients are prepared and dispensed into vials and placed in the auto-
sampler section ready to be injected into the stream of mobile phase. As the mobile phase stream
approaches the column, the auto-sampler injects the reference standard active ingredient/sample
mixture into the mobile phase stream and then the sample/mobile phase mixture then flows
through the column otherwise known as the stationary phase where the separation takes place.
Each analyte resent in the sample interacts with the stationary phase differently. The interaction
depends on the polarity and affinity of the molecules of the analyte to the stationary phase.The
morepolar molecule in the analyte is less strongly attracted to the stationary phase and
40
thereforespends more time in the mobile phase as it moves through the stationary phase while the
less polar molecule in the analyte is more attracted to the non-polar stationary phase and so
spends less time in the mobile phase. The column (stationary phase) is housed in another column
called thecolumn oven which helps to maintain a steady temperature at which the separation is
performed as variation in temperature may affect the retention time of the analyte. The detector
is connected to the stationary phase column. Itgenerates a signal proportional to the amount of
sample component emerging from the column hence allowing for the quantitative analysis of the
sample component. A digital microprocessor and user software control the HPLC instrument and
provide data analysis which is displayed on a display monitor for reading and interpretation by
the analyst. The peaks displayed on the monitor is known as a chromatogram.
EXAMPLE
Product Name : Ampliclox - 500mg
Active : Ampicillin 250mg and Cloxacillin 250mg
Wavelength : 204nm
Column : Octadesyl silica
Flow Rate : 2.0ml per minute
Run Time : 3minutes
Solvent : De-ionized water
Mobile Phase : Acetonitrile (25%), Buffer solution (75%)
41
Ph : 4.5
The ampiclox reference standard and sample are prepared as shown below
Reference standard preparation
Weigh 25mg of ampicillin and cloxacillin reference standard accurately into a beaker and
dissolve with 25ml of de-ionized waters and sonicate for about 5minutes. Pipette 8ml, 6ml, 4ml,
2ml and 1ml into 5 different 10ml volumetric flask respectively and make them up to the mark
with the solvent (de-ionized water). Sonicate again and dispense into vials with each vial well
labelled to indicate the number of mls of the prepared standard solution in it.
Sample preparation
Weigh equivalent of ampiclox and dissolve with 10ml of solvent (de-ionized water) and sonicate
for about 5minutes, filter and dispense into vials.
Both the prepared reference standard and the sample are then handed over to the analyst for
analysis.
42
43
7.0 CHAPTER SEVEN
7.1PHARMACEUTICAL CONTROL LABORATORY (LAB 3)
This is the laboratory that checks the physiochemical parameter of solid oral drugs. The drug
may be in tablet (film-coated, uncoated, sugar coated or enteric coated) or capsule ( Hard gelatin
or soft gelatin). There are machines in this laboratory that provides an environment similar to
that of the human body for these tests to be carried out. They are the disintegration machine and
the dissolution machine. We also have the hardness tester. The idea is to examine the time taken
for a drug to breakdown and the bioavailability of a solid drug dosage in the human body.
The following are the tests carried out in the laboratory
1. Disintegration test
2. Dissolution test
3. Hardness test.
7.2DISINTEGRATION TEST
The disintegration machine is used for this test. The aim is to determine the time taken for the
tablet or capsule to fragment or breakdown in the human body when placed in a liquid in an
environmental condition similar to that in the human body. The following are the various types
of solid drug, the medium, and the acceptable time limit of disintegration for each of them.
1. Uncoated and film coated tablets
Medium – Water
Disintegration time limit – 30minutes
2. Sugar coated tablets
Medium of disintegration – 0.1M HCl
44
Disintegration time limit – 1hour
3. Enteric coated tablets
Medium of disintegration
i. Simulated Intestinal Fluid (S.I.F)
Time – 1hour
Preparation :
S.I.F is prepared by dissolving6.8g of monobasic potassium phosphate in 250ml of water and
then adding 77ml of 0.2 N Sodium Hydroxide and 500ml of distilled water. The resulting
solution is adjusted with 0.2 N HCl to a pH of 6.8 ± 0.1 and finally diluted to 1000ml.
ii. Simulated Gastric Fluid (S.G.F)
Disintegration time – 1hour
Preparation :
Dissolve 2.0 g of NaCl and 3.2 g of purified pepsin in 7.0ml of HCl and water up to 1000ml
with a pH of 1.2
Note : The drug is not expected to breakdown in the simulated intestinal fluid after one hour. It is
then transferred into the simulated gastric fluid after which it is expected to break down within
one hour.
4. Hard gelatin capsule
Medium of disintegration – water
Disintegration time – 30minutes
5. Soft gelation capsule
Medium of disintegration –Acetate Buffer
Disintegration time – 45minutes
45
Preparation(Acetate buffer)
Mix 2.99g of Sodium Acetate monohydrate in 1000ml flask and distilled water plus 1.16ml of
glacial acetic acid with distilled water to obtain 1000ml of solution with an adjusted pH of 4.5 ±
0.05 maintained at 370C ± 2
0C.
Procedure : One tablet or capsule is placed in each of the six tubes of the rack. The rack is then
connected to the disintegration machine and the machine set in motion/operated using the
appropriate medium at 37oc ± 2
oc.
The machine is stopped at 5minutes interval to observe the tablet/capsule in order to know if they
have disintegrated completely before the disintegration time limit specified. If the drug has
disintegrated completely the time is recorded as the time taken for the drug to disintegrate
(disintegration time).
If after the time limit specified there are still 2 or more of the capsules or tablets that did not
disintegrate completely, then the test is repeated for another 6 tablets/capsules. If after the next
six tablets/capsules the drug still did not disintegrate completely, then drug is then handed over
to an analyst to run.
DISINTEGRATION MACHINEDIGITAL THERMOMETHER
46
7.3DISSOLUTIONTEST
This test is carried out in the laboratory to determine the amount of the active ingredient released
from a solid oral dosage form such as tablet or capsule using a dissolution medium.
Procedure
Place the dissolution medium in a vessel of specified apparatus and adjust the temperature of the
medium to 37oc ± 2
oc using a digital thermometer. Place the dosage unit in the apparatus and
operate the apparatus at the specified rate.
After the specified time, withdraw a specimen from the solution and perform an analysis using a
suitable method.
Example
Product Name : Amoxicillin
Active Pharmaceutical Ingredient : Amoxicillin 500mg
Description : Uncoated Tablet
Medium of dissolution : De-ionized water
Volume of medium : 900ml
Speed : 75RPM
Time of dissolution : 60minutes
Temperature of dissolution : 37oc
Wavelength : 272nm
Tolerance : NLT 80%
Apparatus – Filter papers, beaker, 5 25 ml volumetric flasks, Pipette and pipette filler
47
Reagents – Distilled water, De-ionized water.
Absorbance of standard = 0.60006
Dilution factor : 25
100
Absorbance of sample @272nm = 0.58342, 0.48627,0.63766,0.56804,0.56087,0.56725
CALCULATION
Abs of spl × wt of std× vol. of medium × dilution factor × %purity × constant
Abs of std vol. dissolved 1 wt claimed
i. 0.56725 × 22.2 × 900 × 25 × 99 × 100 = 93.49%
0.60006 100 1 10 100 500
ii. 0.56087 × 22.2 × 900 × 25 × 99 × 100 = 92.44%
0.60006 100 1 10 100 500
iii. 0.63766 × 22.2 × 900 × 25 × 99 × 100 = 105.09%
0.60006 100 1 10 100 500
iv. 0.56804 × 22.2 × 900 × 25 × 99 × 100 = 92.62%
0.60006 100 1 10 100 500
v 0.48627 × 22.2 × 900 × 25 × 99 × 100 = 80.14%
0.60006 100 1 10 100 500
vi. 0.58342 × 22.2 × 900 × 25 × 99 × 100 = 96.15%
0.60006 100 1 10 100 500
48
Therefore the sample passed the dissolution test since the percentage of each of the tablets fall
above the tolerance value which is NLT 80%.
DISSOLUTION MACHINE
7.4 HARDNESS TEST
Tablet hardness test is a laboratory technique used by the agency to test the breaking point and
structural integrity of a tablet under conditions of storage, transportation and handling before
usage. The test is only carried out on uncoated tablets.
Procedure
The hardness tester is switched on and allowed to initialize for about 10 minutes. While
initialising, the sample compartment is cleaned with a small brush to remove any drug particle on
it. About 3 tablets are selected randomly from a sachet of the drug sample. One of them is placed
In between the two jaws of the hardness tester machine in a way that it can be compressed by the
jaws. The machine is then operated so that the tablet is squeezed by the jaws until it starts to
49
break. When the tablet fractures, the hardness of the uncoated tablet is displayed on the screen in
Newtons.
HARDNESS TESTER
50
8.0 CHAPTER EIGHT
CONCLUSION AND RECOMMENDATIONS
CONCLUSION
My Student Industrial Work Experience Scheme (SIWES) training with the National Agency for
Food and Drugs Administration and Control (NAFDAC) hasprovided an avenue for me to
understand practical aspects of the theoretical knowledge already acquired in some of the courses
I have offered so far as an undergraduate of Chemistry departmentthrough the necessary
verification tests carried out on cosmetics and drugs to ensure that they are up to the expected
standard for human use. SIWES has made me acquainted to the work environment. I was also
exposed to various laboratory instruments/machines, equipment, professional work methods and
ways to safe guard the work environment in industries and various organizations. The Training
has given me an opportunity to understand some of the basic principles of chemistry which will
further enhance my knowledge of the course.This training also gave me the opportunity to
interact, share knowledge and ideas with other students from different institutions.
RECOMENDATION
TO SIWES
1. The SIWES should endeavor to pay the students industrial visits regularly to ensure that
the students are being trained as expected and not used for purposes other than why they
are there.They should also ensure that the environment is conducive for learning and pay
the students allowances as when due to motivate the students.
2. The training should be well coordinated so that undergraduates can be exposed to the
actual work experience taking place in their respective fields.
3. The Institution should also help in securing placement for students.
TO AGENCY
1. Regular maintenance of instruments and apparatus should be carried out in order to keep
them in good condition
51
2. A more efficient method should be devised for the disposal of waste chemicals used and
workshops should be organized from time to time in order to sensitize workers of the
importance of taking safety precautions when working in the laboratory.
3. NAFDAC should endeavor to organize seminars for their SIWES student intakes in order
to get them familiar with the processes of the laboratories before they start working in the
laboratories because each student has different level of exposure.
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