ANALYSIS LEC - FINALS
ANALYTICAL CONTROL 11. Never leave a reaction unattended. If you
need to leave the lab for a few min.
OBJECTIVE: (restroom break, etc.) Ask someone to
watch your reaction.
To help the Quality Control personnel to conform
12. Always label reagents and flask contents.
with the requirements needed to be GMP
Many organic liquids are clear and
compliant – in their product analysis.
colorless just like water, so are many
QUALITY aqueous solutions such as acids and
bases.
The totality of features or characteristics of a 13. Before starting the analysis read the
product or service that bear on its ability to procedure from the beginning to the end.
satisfy a given need. 14. Document document, document your
analysis results. If it's not written, then
QUALITY CONTROL
you didn't do it!
The mechanisms, processes, techniques and 15. There must be at least two (2) persons
activities necessary to ascertain whether a inside the laboratory when an analysis is
specified standard is being achieved. being performed...
Good Practices in Quality Control includes; ACETAMINOPHEN TABLETS
Basic Laboratory Practices:
1. Clothing - wear proper laboratory gowns Acetaminophen Tablets contains not less
that can protect the analyst. than 90.0% and not more than 110.0% of
2. Hair - long hair should be tied back to the labeled amount of Acetaminophen
keep it from coming into contact with Lab (C8H9NO2)
chemicals or flames. USP Reference standard <11 > - USP
3. Eye Protection - goggles be worn Acetaminophen RS
whenever necessary Identification-
4. Ignition - An open flame may be ignited A. the retention time of the major
only when no flammable solvents are in peak in the chromatogram of the
the vicinity. Assay preparation corresponds to
5. Eating, drinking and smoking are that in the chromatogram of the
prohibited in the laboratory at all times ! Standard preparation as obtained
6. Know the location and operation of: in the Assay.
a. Fire Extinguishers B. Triturate an amount of powdered
b. Safety showers and Eye Tablets equivalent to about 50
c. Wash Stations mg of acetaminophen, with 50 ml
d. Fire Alarm Boxes of methanol and filter: the clear
e. Exit Doors filtrate (test solution) responds to
7. Always remember HOT glassware looks the Thin Layer Chromatographic
exactly the same as COLD glassware, be Identification Test <201 >, a
careful what you touch. solvent system consisting of
8. Many organics don't mix or dissolve in mixture of methylene chloride
water and thus require special waste and methanol (4:1)being used.
containers. Do not pour organics down
the sink!!!! SIGNIFICANT FIGURES USP/NF 29
9. When performing extractions SAVE BOTH
LAYERS (organic and water) until you are "The limits expressed in the monograph
sure which contains the desired product. definitions and tests, regardless of
Can't remember which layer is which? whether the values are expressed as
Add a few drops of water to both from percentage or as absolute numbers are
your wash bottle, the rest will be obvious. considered significant to the last digit
10. Use grease on joints to prevent shown.
“freezing” but not so much that it drips
the joints, except for Teflon stopcocks, Unrounde Rounded Conforms
which are never greased. Glass joints d
which come in contact with Strong Bases" Assay 97.96 % 98.0% Y
(KOH, NaOH etc) need to be greased Limit > 97.92 % 97.9 % N
Failure to clean them promptly after use 98.0 % 97.95 % 98.0 % Y
will result in permanent sealing of the Assay < 101.55 % 101.6 % N
glass surfaces. 101.5 % 101. 46 % 101.5 % Y
, ANALYSIS LEC - FINALS
101.45 % 101.5 % Y Dissolution is the process by which a
Limit 0.025 % 0.03 % N solid enters into solution,
Test < 0.015 % 0.02 % Y The earliest reference to dissolution is
0.02 % 0.027 % 0.03 % N the 1897 article by Noyes and Whitney,
tilled as "The rate of solution of solid
substances in. their own solution.'' The
authors suggested that the rate of
dissolution of solid substances is
determined by the rate of diffusion of a
REFERENCE STANDARD very thin layer of saturated solution that
forms instantaneously around the solid
Substances selected for their high purity, particle. Formed the mathematical
critical characteristics and suitability for Noyes-whitney equation (the traditional
their intended use. mathematical expression for dissolution
Used as a basis for acceptance of test rate).
samples specially in assays Dissolution is more than simple
spectrophotometric methods and measurement of the rate of solubility. It
chromatographic separations. may be accurately described as a
physical lest to predict delivery to a
TYPES OF REFERENCE STANDARDS:
target area ‘in the proper amount at the
Primary Standards - purchased/ provided right time.
by the commissions of the USP, EP, BP Dissolution is defined as the process by
and JP which solid substances enter in solvent to
o ex. USP Reference Standard yield a solution.
Secondary Standards -taken from the Dissolution is the process by which a
innovator drug company/ chemical solid substance dissolves. Fundamentally,
suppliers that have been standardized it is controlled by the affinity between the
against a primary standard solid substance and the solvent.
o ex. In-House Reference Standards The physical characteristics of the
dosage form, the wettability of the
USP ACETAMINOPHEN REFERENCE dosage unit, the penetration ability of the
STANDARD dissolution medium, the swelling process,
the disintegration, and the
Dry a portion over silica gel for 18 Hours disaggregation of the dosage forms are a
before using. Keep container tightly few of the factors that influence the
closed and protected from light. dissolution characteristics of drugs.
For USP Standards “Do not use the
original container as the drying vessel
and do not dry a reference standard
repeatedly at temperature above 25°C
Secondary standards are prepared
according to a Standard Operating
Procedure
The material to be chosen must be of
known reputable source/supplier,
preferably the approved supplier.
The material was received together with
the original COA.
The material passed the tests as per
monograph.
The material was tested versus a primary
standard.
The assay was done at least three (3)
times and the results must be precise.
The Storage Condition must be indicated.
The expiry date is usually one (1) year
but not longer than the expiry date According to Carstensen, the wetting of
stated on COA. the solid dosage form surface controls
the liquid access to the solid surface and
DISSOLUTION is the limiting factor in the dissolution.
ANALYTICAL CONTROL 11. Never leave a reaction unattended. If you
need to leave the lab for a few min.
OBJECTIVE: (restroom break, etc.) Ask someone to
watch your reaction.
To help the Quality Control personnel to conform
12. Always label reagents and flask contents.
with the requirements needed to be GMP
Many organic liquids are clear and
compliant – in their product analysis.
colorless just like water, so are many
QUALITY aqueous solutions such as acids and
bases.
The totality of features or characteristics of a 13. Before starting the analysis read the
product or service that bear on its ability to procedure from the beginning to the end.
satisfy a given need. 14. Document document, document your
analysis results. If it's not written, then
QUALITY CONTROL
you didn't do it!
The mechanisms, processes, techniques and 15. There must be at least two (2) persons
activities necessary to ascertain whether a inside the laboratory when an analysis is
specified standard is being achieved. being performed...
Good Practices in Quality Control includes; ACETAMINOPHEN TABLETS
Basic Laboratory Practices:
1. Clothing - wear proper laboratory gowns Acetaminophen Tablets contains not less
that can protect the analyst. than 90.0% and not more than 110.0% of
2. Hair - long hair should be tied back to the labeled amount of Acetaminophen
keep it from coming into contact with Lab (C8H9NO2)
chemicals or flames. USP Reference standard <11 > - USP
3. Eye Protection - goggles be worn Acetaminophen RS
whenever necessary Identification-
4. Ignition - An open flame may be ignited A. the retention time of the major
only when no flammable solvents are in peak in the chromatogram of the
the vicinity. Assay preparation corresponds to
5. Eating, drinking and smoking are that in the chromatogram of the
prohibited in the laboratory at all times ! Standard preparation as obtained
6. Know the location and operation of: in the Assay.
a. Fire Extinguishers B. Triturate an amount of powdered
b. Safety showers and Eye Tablets equivalent to about 50
c. Wash Stations mg of acetaminophen, with 50 ml
d. Fire Alarm Boxes of methanol and filter: the clear
e. Exit Doors filtrate (test solution) responds to
7. Always remember HOT glassware looks the Thin Layer Chromatographic
exactly the same as COLD glassware, be Identification Test <201 >, a
careful what you touch. solvent system consisting of
8. Many organics don't mix or dissolve in mixture of methylene chloride
water and thus require special waste and methanol (4:1)being used.
containers. Do not pour organics down
the sink!!!! SIGNIFICANT FIGURES USP/NF 29
9. When performing extractions SAVE BOTH
LAYERS (organic and water) until you are "The limits expressed in the monograph
sure which contains the desired product. definitions and tests, regardless of
Can't remember which layer is which? whether the values are expressed as
Add a few drops of water to both from percentage or as absolute numbers are
your wash bottle, the rest will be obvious. considered significant to the last digit
10. Use grease on joints to prevent shown.
“freezing” but not so much that it drips
the joints, except for Teflon stopcocks, Unrounde Rounded Conforms
which are never greased. Glass joints d
which come in contact with Strong Bases" Assay 97.96 % 98.0% Y
(KOH, NaOH etc) need to be greased Limit > 97.92 % 97.9 % N
Failure to clean them promptly after use 98.0 % 97.95 % 98.0 % Y
will result in permanent sealing of the Assay < 101.55 % 101.6 % N
glass surfaces. 101.5 % 101. 46 % 101.5 % Y
, ANALYSIS LEC - FINALS
101.45 % 101.5 % Y Dissolution is the process by which a
Limit 0.025 % 0.03 % N solid enters into solution,
Test < 0.015 % 0.02 % Y The earliest reference to dissolution is
0.02 % 0.027 % 0.03 % N the 1897 article by Noyes and Whitney,
tilled as "The rate of solution of solid
substances in. their own solution.'' The
authors suggested that the rate of
dissolution of solid substances is
determined by the rate of diffusion of a
REFERENCE STANDARD very thin layer of saturated solution that
forms instantaneously around the solid
Substances selected for their high purity, particle. Formed the mathematical
critical characteristics and suitability for Noyes-whitney equation (the traditional
their intended use. mathematical expression for dissolution
Used as a basis for acceptance of test rate).
samples specially in assays Dissolution is more than simple
spectrophotometric methods and measurement of the rate of solubility. It
chromatographic separations. may be accurately described as a
physical lest to predict delivery to a
TYPES OF REFERENCE STANDARDS:
target area ‘in the proper amount at the
Primary Standards - purchased/ provided right time.
by the commissions of the USP, EP, BP Dissolution is defined as the process by
and JP which solid substances enter in solvent to
o ex. USP Reference Standard yield a solution.
Secondary Standards -taken from the Dissolution is the process by which a
innovator drug company/ chemical solid substance dissolves. Fundamentally,
suppliers that have been standardized it is controlled by the affinity between the
against a primary standard solid substance and the solvent.
o ex. In-House Reference Standards The physical characteristics of the
dosage form, the wettability of the
USP ACETAMINOPHEN REFERENCE dosage unit, the penetration ability of the
STANDARD dissolution medium, the swelling process,
the disintegration, and the
Dry a portion over silica gel for 18 Hours disaggregation of the dosage forms are a
before using. Keep container tightly few of the factors that influence the
closed and protected from light. dissolution characteristics of drugs.
For USP Standards “Do not use the
original container as the drying vessel
and do not dry a reference standard
repeatedly at temperature above 25°C
Secondary standards are prepared
according to a Standard Operating
Procedure
The material to be chosen must be of
known reputable source/supplier,
preferably the approved supplier.
The material was received together with
the original COA.
The material passed the tests as per
monograph.
The material was tested versus a primary
standard.
The assay was done at least three (3)
times and the results must be precise.
The Storage Condition must be indicated.
The expiry date is usually one (1) year
but not longer than the expiry date According to Carstensen, the wetting of
stated on COA. the solid dosage form surface controls
the liquid access to the solid surface and
DISSOLUTION is the limiting factor in the dissolution.
