CHAPTER 2- Methods of Analysis in Quantitative Pharmaceutical Chemistry Flashcards
The determination of the VOLUME OF SOLUTION of known concentration required to react with a given amount of the substance to be analyzed
Volumetric Analysis
- Based on some specific physical or chemical property/ properties of the substance being analyzed
- involve instrumental techniques such as chromatography, spectrophotometry, refractometry, polarimetry
Physicochemical Methods
The separation by extraction, precipitation, or other means of the constituent to be determined either in the natural state or in the
form of a definite compound the composition of which is known to the analyst, and the weighing of the resulting product
Gravimetric Analysis
- Those which require a distinct type of technique such as alkaloidal assaying
Special Method
- Done simultaneously
Replicates
- Done at different time
Trials
9 Grades of Chemicals
- Reagent ACS
- Guaranteed Reagent (GR)
- Analytical Reagent (AR) Grade
- Primary Standard
- Purified
- Lab Grade
- USP Grade
- NF Grade
- Technical Grade
High quality chemical for laboratory use (American Chemical Society)
Reagent ASC
Suitable for use in analytical chemistry, products meet or exceed ACS requirement
Guaranteed Reagent (GR)
More or less similar to ACS
Analytical Reagent (AR) Grade
For titration
Primary Standard
Chemicals of good quality where there are no official standards; usually limited to inorganic chemicals.
Purified
A line of solvents suitable for histology methods and general laboratory application
Lab Grade
Chemicals manufactured under CGMP and meet requirements of USP
USP Grade
National Formulary
NF Grade
Suitable for general industrial use
Technical Grade
Undesirable characteristics of a product
Defects
3 Types of Defects
- According to measurability
- According to Seriousness/Gravity
- According to Nature
(2) According to measurability
- Attribute Defect
- Variable Defect
According to measurability
- Cannot be measured by any instrument (ex:
odor, cleanliness)
Attribute Defect
According to measurability
- measured by instruments (ex: weight,
thickness)
Variable Defect
(3) According to Seriousness/Gravity
- Critical Defect
- Major Defect
- Minor Defect
According to Seriousness/Gravity
- Endanger life or property, may render product nonfunctional
(ex: disintegration time)
Critical Defect
According to Seriousness/Gravity
- May render product useless
(ex: cracked bottle)
Major Defect
According to Seriousness/Gravity
- does not endanger life nor affect function
(ex: label)
Minor Defect
(3) According to Nature
- Ocular Defect
- Internal Defect
- Performance Defect
According to Nature
- visible (foreign particulate)
- can be seen in the naked eye
Ocular Defect
According to Nature
- not seen (subpotent)
Internal Defect
According to Nature
- a defect in function
(ex: suppository that does not melt in body temperature)
Performance Defect
4 Sources of Variation (4M’s)
- Material
- Machine
- Method
- Men
- Examine raw materials received
- Conduct physical test for packaging materials
Materials Inspection Section
- Performs physical and chemical analysis
Analytical Laboratory
-Performs microbiological, pharmacological, strerility and toxicity tests
- Conducts environmental monitoring
Biological Testing Laboratory
- Airborne Particulate Cleanliness Classes in Cleanrooms and Clean zones
- Are maintained in areas of parenteral manufacturing
Parenterals - Class 100
- Research development
- Validate procedures
- Develop new assays
- Develop and improve final product
Analytical Development/ Research & Development
- Maintain records
- Investigate complaints
- Maintain and develop SOP
Quality Coordination Office
4 Control Functions
- Analysis Function
- Monitoring Function
- Record, Review and Release Function
- Audit Function
Control Function
- To assure acceptability of product
- All materials are within specifications
Analysis Function
Control Function
- In process testing
- Any deviation must be reported
- Environmental monitoring
Monitoring Function
Control Function
- Batch Record; all records during course of producing quality controlled product
Record, Review and Release Function
Control Function
- Audit Function
Audit Function
Secure a representative samples; sampled from
different parts
Sampling
Finite number of objects selected from a given population
Sample
3 Inspection Methods
- Single Sampling
- Double Sampling
- Triple Sampling
A decision is reached after one sampling
Single Sampling
To avoid mix-ups
Sticker
Yellow
Quarantine
Red
Rejected
Green
Approved
(2) Printed & Packaging Materials
- Primary Packaging Components
- Secondary Packaging
Direct contact with the product
Ex: Caps, capsules, bottles
Primary Packaging Components
Do not come in direct contact
Ex: Labels, inserts and cartons
Secondary Packaging Components
- The date of retest is known as re-assay date
- Monthly or prior to use - highly unstable
materials
Re- assay Dates
6 months - Vitamins, Flavors
12 months - Dyes
24 months - Excipients
Re- assay Dates
Means specific amount produced in a unit time or according to a single manufacturing order during same cycle of manufacture
Batch
A batch; or portion of a batch
Lot
_____ and ______ are witheld from distribution until BATCH CERTIFICATE from FDA is received
Antibiotic and Insulin
2 QC Charts
- Variable Chart
- Attribute Chart
- Use actual records of numerical measurement on a full continuous scale such as meter, grams, liter
Ex: mean and R charts
Variable Chart
- Makes use of discrete data classifying the number of items conforming and falling
Ex: P chart (control chart for
fraction defective)
Attribute Chart
Control Chart consists of:
- Control Solid Line
- Upper Control Limit (UCL)
- Lower Control Unit (LCL)
- Average
- 2 horizontal parallel lines on either sides of the solid line which indicate limits
Control Solid Line
- Normally 3 standard deviation above the centerline
- UCL = Mean + 3 (SD)
Upper Control Limit (UCL)
- Standard deviation below the center line
- LCL = Mean - 3 (SD)
Lower Control Unit (LCL)
