Instrumental Chemical Analysis

Dr. Ahmad Najjar Philadelphia University

Faculty of Pharmacy

Department of Pharmaceutical Sciences

2nd semester, 2018/2019

Introduction

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Course Syllabus

• Course description

This course is devoted to the exploration of the instrumental methods of analysis used to check the purity of raw material and quality control of pharmaceutical preparations; chromatographic methods, spectroscopic methods; UV-Visible, IR, NMR, and Mass spectrometry.

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Course Syllabus

Course code:

0510206

Course title:

Instrumental Chemical Analysis

Course prerequisite:

0510122

Course level:

Second year

Credit hours: 3 hours

Contact hours: 3 hours Lecture time:

Location:

Academic Staff

E-mail address Office

hours

Office number and

location Rank Name

a.najjar@philadelphia.edu.jo 203 Faculty of Nursing Assistant Professor Dr. Ahmad Najjar

Course Syllabus • Course objectives

o Provide the basic tools and facilitate the practical applications of quality control in the production of pharmaceuticals and how pharmaceutical analysis is used to determine the quality of ingredients and the final product.

o Define components and operation procedures, interpret results acquired, and assess the benefits and limitations of different instrumental methods that are critical to drug design and development.

o Identify appropriate instrumental methods that fit certain chemical analysis of a certain pharmaceutical product.

o Design experiment, implement analysis using the relevant chemical literature, process and analyze the data and, effectively, communicate results orally and in writing

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• Textbook:

Chemical Analysis: Modern Instrumentation Methods and Techniques; F. Rouessac and A. Rouessac , John Wiley; second edition (2007).

• Supplementary Textbook:

Undergraduate Instrumental Analysis, J. W. Robinson, Marcel Dekker, sixth edition; (1995).

Course Syllabus

• Assessment components:

• Expected workload

On average, students need to spend 2 hours of study and preparation for each 50-minute lecture/tutorial.

• Attendance policy

Absence from lectures shall not exceed 5. Students who exceed the 5 classes limit without excuse acceptable to and approved by the Dean shall not be allowed to take the final examination and shall receive a mark of zero for the course. If the excuse is approved by the Dean, the student shall be considered to have withdrawn from the course.

20 mark First examination

20 mark Second examination

40 mark Final examination

20 mark Quizzes

100 mark Total

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Course Syllabus Course academic calendar

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# classes

Chapter #: main topics Basic and support material to be covered

1 Introduction Instrumental analytical methods, Analysis steps, instrumental methods characteristics and criteria.

7 Chromatography (Chapter 1: General aspects of chromatography) (Chapter 2: Gas chromatography) (Chapter 3: High-performance liquid chromatography)

Basic principles, Column efficiency, band broadening, van Deemter equation, parameters used in evaluating column performance, instrumentation, types of columns, detectors, and Applications.

6 Ultraviolet and visible spectroscopy (Chapter 9: Ultraviolet and visible absorption spectroscopy)

Basic principles of molecular spectroscopy, Beer-Lambert law, spectra of some representative drug molecules. Applications to pharmaceutical quantitative analysis

1 First Major Examination 4 Infrared spectroscopy

(Chapter 10: Infrared spectroscopy) Basic principles of IR spectroscopy, instrumentation. application of IR in structure elucidation, near IR analysis and its pharmaceutical applications

5 Nuclear magnetic resonance spectroscopy (Chapter 15: Nuclear magnetic resonance spectroscopy)

Basic principles of NMR technique and instrumentation, proton-NMR and carbon-13 NMR. Applications of NMR to structure confirmation in some drug molecules

4 Mass spectrometry (Chapter 16: Mass spectrometry)

Basic principles of mass spectrometry and instrumentation, mass spectra, molecular fragmentation, Applications in pharmaceutical applications and characterization of degradation products

1 Second Major Examination 3 Electroanalytical methods of analysis

(Capter 19: Potentiometric methods) Various types of electrodes ad ion-selective electrodes, Potentiomety and potentiometric titration, Karl Fischer titration, Applications in pharmaceutical analysis.

Final Examination

Introduction • Analytical chemistry is the study of the separation, identification, and

quantification of the chemical components of natural and artificial materials.

Qualitative and Quantitative Analysis

• Pharmaceutical analysis is the application of the knowledge of analytical chemistry to analyze pharmaceutical ingredients in raw materials, finished products or biological matrices.

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Introduction

• Pharmacists need analytical chemistry to isolate, identify and quantify:

active pharmaceutical ingredients in the finished products (QC).

active pharmaceutical ingredients in the stored finished products to

monitor their stability.

drug molecules in biological matrices to study their pharmacokinetics

parameters and their toxicity.

Why we need to study Pharmaceutical Analysis (including instrumental methods)?

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pharmaceutically active substances extracted from

plants and neutral sources.

synthetic molecules produced through drug design

& development process.

pharmaceutical raw materials used in the

pharmaceutical industry.

• Classification of Analytical Methods:

1. Classical (wet-chemical) 2. Instrumental

Introduction

• In all quantitative analytical methods, whether classical or instrumental methods, the analysis is focusing on employing a matter physical extensive property like color intensity, weight, volume, thermal, electrochemical,… etc.

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• Extensive property is directly proportional to the analyte concentration

Signal property = k x Concentration

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Classical Vs. Instrumental

Introduction

Classical Methods Instrumental methods

Reliability and Confident

Low accuracy, low specificity (complex matrix is a challenge)

More confident with trace analysis (high accuracy, precision, selectivity, sensitivity,

Sample size Large Low

Skill required of operator

Easy to use. No need for advance training

Need specific training but easily automated.

Cost and availability of equipment.

Low cost equipments but Each analyte need specific reagents and analytical method

High cost, occupy large space, always need instrument calibration and need reference standard

No. of samples/day and per-sample cost

Low number of samples with moderate cost.

Large number with low cost

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• In the instrumental methods, the instrument converts information stored in the physical or chemical characteristics of the analyte to information that can be manipulated and interpreted by a human. These characteristics needs motivator to be appear.

Analytical Information

Response

System Studied

Analyte Stimulus

Energy Source

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Introduction

• The main instrumental methods that will be studied in this course are:

Spectrophotometric methods: depends on the electromagnetic radiation analyte interaction

Electrochemical methods: depends on electrochemical behavior (Oxidation/Reduction, charge, mobility) of the analyte

Chromatographic methods: Separation and Isolation of analytes depending on structural variation

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To answer this question, we should look at the Analytical Steps… so the first step is to define the problem and off course gathering information about it.

Define the problem

Method selection

Sampling and storage

Preparation of laboratory sample

Dissolution of sample

Separation of interferences

Completion of analysis

Calculation of results

Evaluation of results and their reliability

Introduction

What instrument and analytical method should we use?

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Introduction

Define the problem In order to get clear definition of the problem, we should find answers for the following questions:

1. What accuracy and precision are required?

2. How many samples are available?

3. What sample amount could we obtain?

4. What is the expected concentration range of the analyte?

5. What components of the sample will cause interference?

6. The sample is of what kind (steel, soil, water…)?

7. What are the physical and chemical properties of the sample matrix?

8. When was it released or discharged?

9. Under what circumstances will certain reactions occur?

10. Must the sample be recovered after measurement?

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Introduction For example, suppose we want to analyse Ibuprofen in plasma sample, and we choose High Performance Liquid Chromatography coupled with UV/Vis Detractor instrument to obtain the signal. But…

How could we extract the analyte? (liquid-liquid extraction, solid phase extraction, precipitation extraction, direct injection…etc)

Should we use internal standard? and what it should be? What instrument parameters (column/ mobile phase / temperature/

wavelength… etc) should we use? Should we use calibration curve/ standard addition/ or one-point

evaluation method?

So what method fit the purpose!!

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Even if we choose the suitable available instrument, there are many analytical methods could be found or developed for the analysis of our analyte using that instrument.

Introduction There are several criteria to judge the method

a. Numerical Criteria for Selecting Analytical Methods

Figure of Merit is a numerical expression taken as representing the performance or efficiency of a given device, material, or procedure.

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Introduction b. Other Characteristics to Be Considered in Method Choice

1. Speed 2. Ease and convenience 3. Skill required of operator 4. Cost and availability of equipment 5. Per-sample cost

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