Instrumental Chemical Analysis

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1 L1 Page1 Instrumental Chemical Analysis Dr. Ahmad Najjar Philadelphia University Faculty of Pharmacy Department of Pharmaceutical Sciences 2 nd semester, 2016/2017

2 L1 Page2 Course Syllabus Course title: Instrumental Chemical Analysis Course level: Second year Lecture time: Location: 9311 (section 1), 9414 (section 2 & 3) Course Syllabus Course code: Course prerequisite: Credit hours: 2 hours Contact hours: 2 hours Academic Staff Name Rank Office number and location Office hours address Dr. Ahmad Najjar Assistant Professor 203 Faculty of Nursing a.najjar@philadelphia.edu.jo 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.

3 L1 Page3 Course Syllabus Course objectives o o o 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. 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. Identify appropriate instrumental methods that fit certain chemical analysis of a certain pharmaceutical product. Design experiment, implement analysis using the relevant chemical literature, process and analyze the data and, effectively, communicate results orally and in writing 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).

4 L1 Page4 Course Syllabus Assessment components: First examination Second examination Final examination Quizzes Total 20 mark 20 mark 40 mark 20 mark 100 mark 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.

5 L1 Page5 Course academic calendar Course Syllabus # classe s Chapter #: main topics Basic and support material to be covered 1 Instrumental analytical methods, Analysis steps, instrumental methods 6 Chromatography (Chapter 1: General aspects of chromatography) (Chapter 2: Gas chromatography) (Chapter 3: High-performance liquid chromatography) 5 Ultraviolet and visible spectroscopy (Chapter 9: Ultraviolet and visible absorption spectroscopy) 1 First Major Examination 4 Infrared spectroscopy (Chapter 10: Infrared spectroscopy) 5 Nuclear magnetic resonance spectroscopy (Chapter 15: Nuclear magnetic resonance spectroscopy) 3 Mass spectrometry (Chapter 16: Mass spectrometry) 1 Second Major Examination 3 Electroanalytical methods of analysis (Capter 19: Potentiometric methods) 3 Statistical treatment of analytical data (Chapter 22: Basic statistical parameters) characteristics and criteria. Basic principles, Column efficiency, band broadening, van Deemter equation, parameters used in evaluating column performance, instrumentation, types of columns, detectors, and Applications. Basic principles of molecular spectroscopy, Beer-Lambert law, spectra of some representative drug molecules. Applications to pharmaceutical quantitative analysis Basic principles of IR spectroscopy, instrumentation. application of IR in structure elucidation, near IR analysis and its pharmaceutical applications Basic principles of NMR technique and instrumentation, proton-nmr and carbon-13 NMR. Applications of NMR to structure confirmation in some drug molecules Basic principles of mass spectrometry and instrumentation, mass spectra, molecular fragmentation, Applications in pharmaceutical applications and characterization of degradation products Various types of electrodes ad ion-selective electrodes, Potentiomety and potentiometric titration, Karl Fischer titration, Applications in pharmaceutical analysis. Significant figures, Errors, Accuracy and precision, reporting of results. Final Examination

6 L1 Page6 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.

7 L1 Page7 Why we need to study Pharmaceutical Analysis (including instrumental methods)? Pharmacists need analytical chemistry to isolate, identify and quantify: 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. 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.

8 L1 Page8 Classification of Analytical Methods: 1. Classical (wet-chemical) 2. Instrumental 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. Extensive property is directly proportional to the analyte concentration Signal property = k x Concentration

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10 L1 Page10 Classical Vs. Instrumental Reliability and Confident Classical Methods Low accuracy, low specificity (complex matrix is a challenge) Sample size Large Low Skill required of operator Cost and availability of equipment. No. of samples/day and per-sample cost Easy to use. No need for advance training Low cost equipments but Each analyte need specific reagents and analytical method Low number of samples with moderate cost. Instrumental methods More confident with trace analysis (high accuracy, precision, selectivity, sensitivity, Need specific training but easily automated. High cost, occupy large space, always need instrument calibration and need reference standard Large number with low cost

11 L1 Page11 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. Stimulus Analyte Response Energy Source System Studied Analytical Information

12 L1 Page12 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

13 L1 Page13 What instrument and analytical method should we use? To answer this question, we should look at the Analytical Steps 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 so the first step is to define the problem and off course gathering information about it.

14 L1 Page14 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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17 L1 Page17 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. 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!!

18 L1 Page18 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.

19 L1 Page19 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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