Pharmacy Analytical Chemistry II

Laboratory techniques in Pharmacy, organic chemistry and inorganic chemistry

Expository lectures with audiovisual and interactive resources between student and teacher, with

use of theoretical-practical lessons to reinforce the understanding of theoretical syllabus

Students will be monitored throughout each semester with questions as a complement of

education.

Are offered two hours per week, with pre-defined schedule with the student.

Are also delivered to each student teaching holders of all matter taught or bibliographical

references recommended for discipline, at the beginning of the semester.

The curricular unit of analytical chemistry in pharmacy I aims to provide the student an adequate

knowledge of theoretical principles, practices and application components of instrumental

methods of analysis, essential to the performance of laboratory activities, having as main

objective the application of new technologies in the area of Pharmacy, your validation, as well as

in the area of investigation.

Also wants to enable and empower the learner on programming steps of developing an analytical

method, as well as in the selection of this, in the face of specific requirements, such as:

specificity, sensitivity, detection limit, selectivity, reproducibility and matrix interference, defining

further indicates the factors that lead to the choice of a particular method of analysis.

Competencies to develop:

-Understanding of the nature, objectives and applications of instrumental methods of analysis;

-Acquisition of knowledge and skills in the application of analytical methods in solving analytical

problems;

– Ability to define/select experiences and procedures in obtaining results;

-Ability to identify the conditions of applicability of various quantitative and qualitative analytical

methods;

-Determination of the concentration of various analytes by classical methods and instruments;

– Ability to handle and interpret analytical results.

Theoretical matrix

1 UV-VISIBLE SPECTROSCOPY – 4h

1.1. Basic principles and instrumentation

1.2. The process of absorption and emission of ultraviolet-visible radiation

1.3. Photoelectric effect

1.4. Color

1.5. Electromagnetic Spectrum

1.6. Absorption and emission spectra of hydrogen

1.7. Electronic transitions

1.8. Ultraviolet-visible spectrophotometers

1.9. Beer-Lambert

1.10. Analytical applications

INFRARED SPECTROSCOPY 2 – 4 hours

2.1. Basic principles and instrumentation

2.2. The process of absorption of infrared radiation

2.3. Vibration modes

2.4. Applications of Infrared spectrum

2.5. Bands

2.6. Dispersive Espetrofotometros

2.7. Fourier transform Espetrofotometros

2.8. Sampling Techniques

2.8.1. Transmission techniques

2.8.2. Reflectance techniques

2.9. Analysis Infrared spectra

2.10. Analytical applications

3 SPECTROSCOPY OF NUCLEAR MAGNETIC resonance – 2 hours

3.1. Basic principles and instrumentation

3.2. Nuclear spin states

3.3. Energy absorption

3.4. The resonance phenomenon

3.5. Chemical shift and protection

3.6. Analytical Applications

4. SPECTROSCOPY ATOMIC ABSORPTION AND EMISSION – 4 hours

4.1. Basic principles and instrumentation

4.2. Chemical, physical and spectral interferences

4.3. Quantification

4.4. Atomic absorption spectroscopy flame

4.5. Atomic absorption spectroscopy with graphite furnace

4.6. Atomic emission spectroscopy Flame (ICP)

4.7. Analytical applications

5 Capillary Electrophoresis – 2 hours

5.1. Basic principles and instrumentation

5.2. Resolution and efficiency

5.3. electroosmosis

5.4. Capillary zone electrophoresis (CZE)

5.5. Isoelectric focusing (IEF)

5.6. Capillary gel electrophoresis (CGE)

5.7. “Isotachophoresis” capillary (ISCO)

5.8. Micellar electrokinetic capillary chromatography (MEKC)

5.9. analytical applications

Im-12-07-B3 5

6 ELEMENTAL ORGANIC ANALYSIS – 2 hours

6.1. Basics principles

6.2. Organic and inorganic compounds

6.3. Methods used in organic elemental analysis

6.4. Qualitative Analysis

6.5. Quantitative elemental analysis

6.6. Organic elemental analysis to obtain empirical formulas and molecular

7.CHROMATOGRAOHY – 8 hours

7.1. Basic principles

7.2. Liquid chromatography

7.2.1. Paper choromatography

7.2.2. Thin layer choromatography(TLC)

7.2.3. Column choromatography

7.2.3.1. Liquid-liquid choromatography

7.2.3.2. Solid-liquid choromatography

7.3. Gas chromatography

7.3.1. Instrumentation

7.3.2. Gas injection systems

7.3.3. Packed columns vs. capillary columns

7.3.4. Substrates and liquid phases

7.3.5. Gas-solid choromatography

7.3.6. Liquid gas choromatography

7.3.7. Adsorption choromatography

7.3.8. Partition choromatography

7.3.9. Types of detectors

7.4. High Performance Liquid Chromatography (HPLC) and Ultra Performance Liquid Chromatography

7.4.1. Iinstrumentation

7.4.2. Columns: types, applications and selection criteria

7.4.3. Types of interaction between the mobile phase and the stationary phase

7.4.3. Chemically bonded stationary phases

7.4.2. Normal phase chromatography and reverse phase

7.4. Analytical applications

Practice matrix

1 UV-Visible Spectroscopy – 12 hours

1.1. Absorption spectrum of the copper sulfate

1.2. Determination of nitrate and nitrite in waterS

1.3. Absorption spectra of the paracetamol

1.4. Spectrophotometric determination of caffeine

2 Chromatography – 21 hours

2.1. Separation and identification of phenolic acids in plant extracts by thin layer chromatography

2.2. Identification of caffeine by thin layer chromatography

2.3. Determination of the amount of caffeine by HPLC-UV

2.4. Simultaneous determination of acetaminophen and ibuprofen by HPLC-UV

2.5. Determination of captopril in tablets by HPLC-UV

2.6. Simultaneous separation of estrogens and their quantification by UPLC-FLR

2.7. Determination of fluoxetine  by UPLC-MS

3. Quantitative analysis – 6 hours

3.1. Determination of antiacid mass in a commercial sample

3.2. Separation of components of an analgesic and its quantification

NAO

Primary Bibliography:

-Skoog D.A., Nieman T.A., Holler F.J., Princípios de Análise Instrumental, 5ª edição, Bookman

– Skoog D.Aa., West D.M., Holler F.J., Fundamentals of analytical chemistry, 7ª ed., Saunders

College Publishing, 1996

– Skoog D.A., West D.M., Holler F.J., Analytical chemistry – An introdution, 7ª ed., Saunders

College Publishing

– Pombeiro A.J.L.O. Técnicas e operações unitárias em química laboratorial. 2ª ed. Fundação

Calouste Gulbenkian. Lisboa 1991

Secondary Bibliography:

– Lobinson J. W., Undergraduate instrumental analysis, 5ªed, revised and expanded, Marcel

Dekker inc

– Gnçalves M.L. S. S., Métodos instrumentais para análise de soluções, 3ªed., Fundação Calouste

Gulbenkian, lisboa

– Skoog D. A., leary J. J., Principles of instrumental analysis, 4ªed, Harcourt brace college

publishers

– Christian G. D., o’Reilly J. E., Instrumental analysis, 2ªed, allyn and bacon, inc.

– Alexéev v. Análise qualitativa. Lopes da silva editora, Porto, 1982.

– Alexéev v. Análise quantitativa. 3ª ed. Lopes da silva editora, Porto, 1983.

– Vogel R. I., Quantitative chemical analysis. 15ª ed. Longman scientific & technical, New

York,1989

– Kellner R., Mermet J. M., Otto M., Widmer H. M., Analytical chemistry, Widel-vch

– Cristian Gary D., Analytical Chemistry, 5ª edition

Willard H., Merrit L., Dean J., Análise instrumental, 2º ed., Fundação Calouste Gulbenkian. Lisboa

– Brett C. M. A., Brett A.M.O., Electrochemistry principles, methods and applications, Oxford Univ.

Press, Oxford, 1993

– Brett C. M. A., Brett A.M.O., Electrochemistry principles, methods and applications, science

publication, Oxford, 1996

– Brett C. M. A. Brett, A.M.O., Electroanalysis, Oxford univ. Press, Oxford, 1998

– Rousseac F., rousseac A., Chemical analysis – Modern instrumentation methods and

techniques”, Wiley, 2000

– Currell G. Analytical instrumentation – performance, characteristics and quality”, Wiley, 2000

– Mahan Bh. Química, um curso universitário. 2ª ed. Edgar blücher ltda., São Paulo, 1972

– Morrison R, Boyd R. Organic chemistry. 2ª ed. Allyn and bacon inc., Boston, 1973

– Pavia, Dl, Lampman, Gm, Kriz GS. Introduction to spectroscopy. Saunders college, Philadelphia 1986Eq