WEEK NO.

3
Mariano Marcos State University
College of Health Sciences
Pharmacy Department
City of Batac 2906 Ilocos Norte

PHCHM 104: PHARMACEUTICAL ANALYSIS 2 (INSTRUMENTAL METHODS OF ANALYSIS)

2nd Semester of A.Y. 2020-2021

Compendial Requirements for Pharmaceutical Products:

Chapter 3: Statistical and Stability

Learning Input 1

Statistical Quality Control

Standard Deviation
 A statistical term used to measure the amount of variability or dispersion around an
average.

Gaussian Curve or Bell curve

 68% of scores are within one standard deviation of the mean

 95% of scores are within 2 standard deviation of the mean.
 99.7% of scores are within 3 standard deviation of the mean

1. Twenty sets of ten tablets were weighed during compression at thirty minutes intervals,
calculate the upper control limit and lower control limit.
a. Use the formula:

X (mg)

373.9 3.65 13.3225

Pharmaceutical Analysis 2: Instrumental Analysis 1

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
 WEEK NO. 3

381.5
374.1
365.1
370.0
365.8
367.9
370.0
374.1
369.7
365.1
370.6
368.0
372.8
371.1
365.2
366.9
372.5
370.3
370.4
∑=
=

𝑈𝐶𝐿 = + 3𝛿

𝐿𝐶𝐿 = − 3𝛿

b. Using the table below, calculate the standard deviation using the formula:

Pharmaceutical Analysis 2: Instrumental Analysis 2

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
 WEEK NO. 3

R = range
D = divisor for the sample size used

Sample Size Divisor Sample Size Divisor

2 1.1 10 3.1
3 1.7 15 3.5
4 2.1 20 3.7
5 2.3 30 4.0
6 2.7 50 4.5
8 2.8 100 5.0
9 3.0 500 6.0

2. The volume of 5 vials was determined during the filling of an injectable. Determine the UCL
and LCL using the formulas:

No. of Volume (ml) of vials every 30 min.

R
Inspection A B C D E
1 10.5 10.3 10.2 10.6 10.7 10. 46 0.50
2 10.4 10.0 10.3 10.2 10.1
3 10.1 9.8 9.9 9.6 9.7
4 9.8 9.8 10.0 10.2 10.1
5 10.6 10.5 10.5 10.5 10.4
6 10.7 10.5 10.6 10.7 10.9
7 10.7 10.3 10.5 10.4 10.4
8 10.8 10.2 10.7 10.8 10.9
9 10.0 10.3 10.4 10.1 10.0

Pharmaceutical Analysis 2: Instrumental Analysis 3

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
 WEEK NO. 3

10 10.0 10.0 10.0 10.4 10.3

11 9.8 9.9 9.8 9.8 9.9
12 10.7 10.6 9.6 10.9 10.5
13 10.1 10.6 10.4 10.7 10.3
14 10.5 10.9 10.5 10.6 10.4
15 10.3 10.3 10.2 10.5 10.3

Factors for Chart Factors for

Sample Size
D3 D4 Chart (A2)

2 0.00 3.27 1.88

3 0.00 2.57 1.02
4 0.00 2.28 0.73
5 0.00 2.11 0.58
6 0.00 2.00 0.48
7 0.08 1.92 0.42
8 0.14 1.86 0.37
9 0.18 1.82 0.34
10 0.22 1.78 0.31

Stability

Stability is the extent to which a product retains within specified limits and throughout
its period of storage and use the same properties and characteristics that it possessed at the
time of its manufacture.

Five types of stability concerns:

• Physical
• Clarity and color of solution
• Moisture

Pharmaceutical Analysis 2: Instrumental Analysis 4

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
 WEEK NO. 3

• Crystal modification
• Particle size

• Chemical
• Hydrolysis
• Oxidation
• Reduction
• Photolysis

• Therapeutic Activity
• Potency

• Toxicological Activity
• No significant increase in toxicity occurs.

Factors:
• Temperature
• Humidity
• pH
• Excipient
• Packaging component

Learning Output 2

Instability evidences in different dosage forms

Solid dosage forms

Hard and soft gelatin capsules
 Hardening or softening of the shell, release of gas such as a distended paper seal.

Coated tablets
 Cracks, mottling or tackiness in the coating and clumping of tablets.

Uncoated tablets
 Cracks, mottling, swelling, discoloration and fusion between tablets.

Dry powders and granules

 Caking into hard masses or discoloration

Effervescent tablets, granules or powders

 Swelling of the mass or development of gas pressure.

Pharmaceutical Analysis 2: Instrumental Analysis 5

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
 WEEK NO. 3

Liquid dosage forms

Solutions, elixirs and syrups
 Precipitation or formation of gases or evidence of microbial growth.

Emulsions
 Breaking (separation of oily phase that is not easily dispersed)

Suspensions
 A caked solid phase that cannot be re-suspended after shaking or presence of large
particles.

Sterile liquids (parenteral solutions or ophthalmic solutions)

 Presence of any sign of contamination like change in color, cloudiness and surface film.

Tinctures
 Precipitation

Semisolid dosage forms

Creams
 Emulsion breakage, crystal growth, shrinking due to evaporation of water and gross
microbial contamination.

Ointments
 Change in consistency, separation of excessive amount of liquids and formation of
granules.

Suppositories
 Excessive softening ,dryness or hardening

Pharmaceutical Analysis 2: Instrumental Analysis 6

This study source was downloaded by 100000869050689 from CourseHero.com on 07-12-2023 07:11:48 GMT -05:00

https://www.coursehero.com/file/82196883/PCHM-104-CHAPTER-3pdf/
Powered by TCPDF (www.tcpdf.org)