Introduction to Pharmaceutical Analysis 1: Overview, Definitions, and Philippine Market Trends, and Methods

Course Overview and Syllabus

• Course Title: Pharmaceutical Analysis 1

• Course Facilitator: Ernest Van Rito, RPh

• Institutional Information: College of Pharmacy (Valenzuela, Quezon City, Antipolo, Pampanga, Cabanatuan, Laguna)

• Learning Outcomes:

  • Define Pharmaceutical Analysis.

  • Define terms related to pharmaceutical analysis.

  • Discuss the general types of analysis.

Weekly Topic Schedule

• Week 1: I. Orientation (A. VMV, B. Introduction - Terms)

• Week 2: Methods of Analysis

• Week 3: Official References (Official Compendia, Parts, How to use the Monograph)

• Week 4: Volumetric Analysis

• Week 5: Titrimetric Method Overview and Volumetric Method (Cont.)

  • A. Terminologies

  • B. Types Based on nature of titrant used

  • C. Types based on reactions

  • D. Volumetric Solutions

• Week 6: Volumetric Method: A. Neutralization – Aqueous

• Week 7: Volumetric Method: A. Neutralization – Non-Aqueous

• Week 9: C. Complexation

• Week 12: Midterm Examination

• Week 13: Gravimetric Method

• Week 14-15: Pharmacopeial Analysis of Crude Drugs

  • A. Ash

  • B. Water Content Determination

  • C. Extractives - Alkaloids

• Week 16: Analysis of Fats, Fixed Oils and Fatty Substances

• Week 17: Analysis of Volatile Oils

• Week 18: Final Examination

Required and Reference Literature

• Textbook: Knevel, A.M. and Digangi, F.E., Jenkin’s Quantitative Pharmaceutical Chemistry. USA: Mc Graw Hill, 1977.

• Secondary References:

  • Watson, David G., Pharmaceuticals Analysis: A Textbook for Pharmacy Students and Pharmaceutical Chemists, 4th ed. Singapore: Elsevier, 2017.

  • Remington’s Pharmaceutical Sciences, (2013) Philadelphia: Lippincott William and Wilkin.

  • WHO Expert Committee on Specifications for Pharmaceutical Preparations. Geneva: World Health.

  • British Pharmacopeia, 2017.

  • The United States Pharmacopeia (USP 40) : NF 35: The National Formulary. Rockville, Md.: United States Pharmacopeial Convention, 2017.

  • Handbook of Modern Pharmaceutical Analysis (2011) Amsterdam; Boston: Academic Press/Elsevier.

  • Harris, D.C., Quantitative Chemical Analysis, 9th ed. New York: W.H. Freeman, 2015.

Fundamental Definitions and Concepts

• Drug:

  • General Definition (PharmaXChange.info): Any substance (except food and water) when taken into the body alters the body’s function either physically and/or psychologically.

  • Therapeutic Definition: Any substance, other than food, used in the prevention, diagnosis, alleviation, treatment, or cure of disease.

  • Official Regulatory Definition:

    • A substance recognized by an official pharmacopoeia or formulary.

    • A substance intended for use in the diagnosis, cure, mitigation, treatment, or prevention of disease.

    • A substance (other than food) intended to affect the structure or any function of the body.

• Pharmaceutical (Product): A finished dosage form (e.g., tablet, capsule, or solution) that contains an active pharmaceutical ingredient, generally (but not necessarily) in association with inactive ingredients.

• Active Pharmaceutical Ingredient (API): Any substance or mixture of substances intended to be used in the manufacture of a drug (medicinal) product and that, when used in the production of a drug, becomes an active ingredient. APIs produce pharmacological activity or other direct effects in diagnosis, cure, mitigation, treatment, or prevention of disease or affect the structure or function of the body.

• Excipients: Components of the finished product other than the API. Examples include:

  • Fillers

  • Colorants

  • Flavorants

  • Solvents

  • Preservatives

Pharmaceutical Industry Landscape in the Philippines

Top Pharmaceutical Companies

• Pfizer

• AstraZeneca Philippines

• Eli Lilly and Company

• GlaxoSmithKline

• Merck, Sharp and Dohme

• Novartis

• Roche

• Sanofi-Aventis Philippines

• United Laboratories

• Wyeth

• Abbott

• Johnson & Johnson

• Boehringher Ingelheim

• Bristol Myers Squibb

• Bayer

• Pascual Laboratories

• Schering Plough

• GV International

Top 10 Ethical/Prescription Brands (Sept Moving Annual Total)

1. Novarsc (Pfizer): Hypertension (Generic: Amlodipine)

2. Ventolin (Glaxo-SK): Asthma (Generic: Albuterol)

3. Plavix (Sanofi-Aventis): Thrombosis (Generic: Clopidogrel Bisulfate)

4. Augmentin (Glaxo-SK): Infection (Generic: Amoxicillin + Clavulanate)

5. Neobloc (GX International): Hypertension (Generic: Metoprolol)

6. Lipitor (Pfizer): Hyper-cholesterolemia (Generic: Atorvastatin)

7. Tazocin (Wyeth): Infection (Generic: Tazobactam)

8. Zegen (United American-UL): Infection (Generic: Cefuroxime Axetil)

9. Plendil ER (Astra Zeneca): Hypertension (Generic: Felodipine)

10. Seretide (Glaxo-SK): Asthma (Generic: Fluticasone + Salmetrol)

Top 10 OTC Brands (Moving Annual Total)

1. Ceelin (Pediatrica): Vitamin Supplement

2. Solmux (Westmont): Cough

3. Neozep (Myra): Cold Relief

4. Biogesic (Biomedis): Pain Relief

5. Enervon C (United American): Vitamin Supplement

6. Alaxan (Therapharma): Pain Relief

7. Myra E (Myra): Vitamin Supplement

8. Xenical (Roche): Weight Management

9. Centrum (Wyeth): Vitamin Supplement

10. Cherifer (GX Pharma): Vitamin Supplement

Pharmaceutical Formulations and Quantitative Compositions

Example 1: Tablet Formulation

• Glibenclamide: $5.0\,mg$

• Croscarmellose sodium: $25.0\,mg$

• Corn starch: $25.0\,mg$

• Magnesium stearate: $3.0\,mg$

• Color-Pink lake blend: q.s. (quantum satis)

• Fast-dissolving granulation: $250.0\,mg$

• Aspartame sodium: $9.5\,mg$

• American mint: $3.5\,mg$

• Silicon dioxide: $3.0\,mg$

Example 2: Capsule Formulation (Rx for 100 Capsules)

• Ketoprofen: $1.25\,g$

• Riboflavin: $10\,g$

• Caffeine: $3\,g$

• Sodium bicarbonate: $20\,g$

• Silica gel: $250\,mg$

Example 3: Percent by Weight Composition

• Rosuvastatin Calcium: $1.00\%$

• Diluent: $5.00\%$

• Effervescent couple: $80.00\%$

• Binder: $5.00\%$

• Lubricant: $0.50\%$

• Sweetener: $4.00\%$

• At least 1 other excipient: $4.50\%$

• Total: $100\%$

Pharmaceutical Analysis: Core Definition and Framework

Definitions

• General Analysis: A detailed examination of anything complex in order to understand its nature or to determine its essential features (a thorough study).

• Pharmaceutical Analysis:

  • A branch of practical chemistry involving a series of processes for the identification, determination, quantification, and purification of a substance.

  • Used for the separation of components from a mixture.

  • Used for the determination of the structure of compounds.

  • Application of analytical procedures to determine the purity, safety, and quality of drugs and chemicals.

• Related Terms:

  • Assay: Specifically refers to the testing of a metal or drug to determine its ingredients or quality.

  • Composition of matter: The chemical makeup of a substance.

Major Types of Analysis

1. Qualitative Chemistry:

   • Question: "What is in the sample?"

   • Focus: Identification, determination of composition, and ascertainment of impurities.

2. Quantitative Chemistry:

   • Question: "How much is in the sample?"

   • Focus: Determination of the proportion of components in a substance.

Qualitative to Quantitative Transformation Exercise

• Qualitative Statement: "They eat all the time."

• Qualitative Statement: "The president is very much liked."

• Qualitative Statement: "She saves a lot from her daily allowance."

• Qualitative Statement: "The cruise ship she saw was huge."

• Qualitative Statement: "The cat is very fat."

• Note: In pharmaceutical context, practitioners must provide exact quantitative statements for these observations.

Applications of Analysis in Pharmacy

• Purity and Quality: Analysis of drugs and chemicals used in clinical practice.

• Broad Application: Applied throughout industry, medicine, and the environment.

• Human Physiology: Analysis of chemical constituents found in the human body.

• Biological Systems: Analysis of medicinal agents and their metabolites found in biological systems.