Introduction to Pharmaceutical Analysis Flashcards
Methods for determining the chemical composition of samples of matter
Analytical Chemistry
yields information about the identity of
atomic or molecular species or the functional groups in the sample
Qualitative Method
provides numerical information as to the
relative amount of one or more of these components.
Quantitative MEthod
The process of a quantitative determination of a
chemical substance from a given sample
Asay
Types of Method of Drug Analysis
Nature of Sample
Size of Sample
Extent of Analysis
What is the classifications of nature of sample
Physical
Chemical
Biological
Instruments, Device
Physical
Reagents, Compounds, substances
Chemical
Living organisms, urine, animals, microorganisms
Biological
What are the classifications of Size of Sample?
Macroanalysis
Semi-microanalysis
Microanalysis
Submicroanalysis
Ultramicroanalysis
0.1 g or more
Macroanalysis
0.1 g - 1 g
Semi-microanalysis
0.01 g - 0.1 g
Microanalysis
0.001 g - 0.01 g
Submicroanalysis
<0.001 g
Ultramicroanalysis
The sum of total of the organised arrangements made with the object of ensuring that all APIs are of the quality required for their intended use and quality systems are maintained
Quality Assurance
Checking or testing that specifications are met
(PIC/s cGMP 2018)
Quality Control
Ensures the safety, efficacy, stability and purity
of raw materials and drug products.
Quality Control
• identification, determination, quantification and
purification of a substance;
• separation of the components of a solution or
mixture; or
• determination of structure of chemical compound
Pharmaceutical analysis
analysis of raw materials active pharmaceutical ingredients (APIs), intermediates, excipients, pharmaceutical substances and finished products
Pharmaceutical Analysis
Classification of Analytical Methods of Techniques
Separation
Qualititative Analysis
Quantitative Analysis
What are the classical methods of separation techniques
Precipitation
Extraction
Distillation
What the classical methods of Qualititative analysis
Chemical tests
B.P.
M.P
Solubility
Odor,
Optical activitt
Refractive index
What is the classical methods of the technique quantitative analysis
Titrimetry, Gravimetry, Coulometry
what are the instrumental methods of separation techniques
Chromatography,
electrophoresis
what are the instrumental methods of the technique quantitative analysis
UV/Vis spectrometry,
infrared spectrometry,
MS, NMR spectrometry
what are the instrumental methods of quantitative analysis
Potentiometry,
voltammetry,
spectrophotometry, AAS,
thermometric methods,
kinetic methods
Securing or getting a representative sample from
a given population
Sampling
what are the two types error
Indeterminate
Determinate
Aka Random Error
indeterminate
Uncontrolled variable
Indeterminate
inherent error
indeterminate
Intangible
Indeterminate
Systematic Error
Determinate error
Flaw in the equipment or design of the experiment
Determinate error
Reproducibility of the result
Precision
Usually expressed as average deviation, standard
deviation or range.
Precision
difference between the largest and smallest
value.
Range
describes how close a measured value is to the
“true” value
accuracy
Difference between the mean value and true value
Absolute Error
Absolute error divided by the true value
Relative Error
Enumerate the classical method of trimetry
Neutralization
Redox
Complexation
Volumetric Precipitation
Enumerate general or classical mehods
Trimetry
Gravimetry
a volume of a solution of known concentration consumed during analysis is taken as a measure of the amount of active constituent in a sample being analysed
Titration
measuring the volume of known concentration needed to react with analyte
Volumetric Titrations
Mass instead of volume
Gravimetric Titrations
measure time require for complete electrochemical reaction
Coulometric Titrations
standard solution of known concentration
Titrant
substance to be determined
analyte
Organic substances (acids/bases) capable of existing in two
forms of different color depending on the pH
Indicator
Theoretical point reached when the titrant and analyte
are chemically equivalent
Equivalence Point
When a physical change occurs that is associated with the condition of chemical equivalence
End point
weight of the substance chemically equivalent to 1mL of a
standard solution.
Titer
Weight of a substance in gram that is chemically equivalent
to 1 gram-atom of hydrogen.
Gram-equivalent weight
Titrant is directly added to analyte until the reaction goes to
completion
Direct Titration
addition of excess titrant, the volume of which that did not
react with the analyte is then titrated (residual or back
titration)
Residual Titration
Objectives
• To find out the effect of the impurities
• To determine the excess standard solution necessary to
establish the end-point
Titration with Blank Test
enumerate other types of titration
Indirect Titration
Double Residual Titration
What are some detection methods
Visual
Instrumental
Appearance/Disappearance of color
Visual
Change in color
Visual
Appearance and disappearance of turbidity
Visual
Colorimeters, turbidimeters, spectrophotometers
Instrumental
Potentiometer
Instrumental
for general industrial use
technical grade/commercial
chemicals manufactured under current GMP
and which meet the requirement of USP/NF
USP/NF
high quality chemical for laboratory use
(Reagent A.C.S. – American Chemical Society)
Analytical
products of purity suitable for use in general applications
Chemically pure
analytical reagent of exceptional purity that is specially manufactured for standardizing volumetric solutions and preparing reference standards.
Primary Standard grade
What are the grades of reagents?
Technical Grade/Commerical
USP/NF
Analytical
Chemically pure
Primary Standard grade
Determination of exact concentration (Normality or
Molarity) of a solution
Standardization
• Highly purified compound
• Serves as a reference material for a titration and in other analytical
methods
• Used to standardize the volumetric solutions (VS)
Primary Standard
• Purity has been determined by chemical analysis
• Serves as the working standard material for titrations and for other
analyses
• Concentration is subject to large uncertainty against 1O standard
Secondary Standard
What are concentration Expressions?
Molarity
Normality
Percent Strength
MW divided by the number of electrons shared by
atoms in a molecule (TOTAL POSITIVE CHARGE)
Equivalent Weight
