The subject Analytical Chemistry is taught in the first quarter of the 2nd year of the Degree in Pharmacy. This is a mandatory four-month subject that consists of a total of 9 ECTS credits.



In order to properly follow this subject, it is recommendable that students have acquired previous knowledge about some aspects of this matter in other subjects from the first year of the degree, including knowledge in statistics acquired in the subject Mathematics and Statistics, in formulation and chemical equilibria in the subject General and Inorganic Chemistry, knowledge in the physicochemical properties of systems in the subject Physical Chemistry or in reactivity and systematics of functional groups in the subject Organic Chemistry. In this connection, taking this subject will allow for the acquisition of knowledge which may be applied in other subjects such as Clinical Biochemistry, Pharmacognosy, Pharmacology and Pharmaceutical Technology.

Subject-specific competences:

A1. To properly use the basic terminology of Analytical Chemistry.

A2. To predict the possible chemical equilibria in aqueous solutions, and to make and interpret the different types of logarithmic diagrams to deduce the concentrations of the different species in a system when it reaches equilibrium.

A3. To select, suggest and evaluate classic analysis techniques, volumetry and gravimetry, to solve specific problems within the pharmaceutical field.

A4. To suggest and develop the different stages of the general analysis process focusing on a particular analytical problem. Application to the resolution of practical cases of pharmaceutical interest.

A5. To select the most appropriate separation technique to improve sensitivity and selectivity of analytical measurements.

A6. To know the principles and procedures necessary for collecting and preparing samples based on the analyte(s) to be determined, and the features of the matrix where it is located.

A7. To select, suggest and evaluate the application of instrumental techniques in the analytical measurement process.

A8. To understand the interest of chromatographic processes as dynamic separation techniques on-line with detection systems.

A9. To perform sample analysis and data interpretation.

A10. To perform bibliographic searches in different databases, scientific journals and books, interpreting the obtained information to solve practical cases related to Analytical Chemistry in the pharmaceutical and health field.



Specific and transversal competences of the degree worked on with this subject:

1-. To do hygienic-sanitary analyses, especially those related to food and the environment.

2-. To design, apply and evaluate reagents, methods and clinical analytical techniques, knowing the fundamentals of clinical analyses and the features and contents of laboratory diagnostic reports.

3-. To identify, design, obtain, analyse, control and produce drugs and medicines, as well as other products and raw materials of health interest for human or veterinary use.

4-. Recognize one's own limitations and the need to maintain and update professional competence, paying special importance to self-learning of new knowledge based on available scientific evidence.

5-. To know how to apply the scientific method and to acquire skills in the management of legislation, sources of information, bibliography, development of protocols and other aspects that are considered necessary for the design and critical evaluation of preclinical and clinical trials.



Transversal Competences of the UPV/EHU:

- Autonomy and self-regulation

- Social commitment

- Ethics and professional responsibility

- Critical thinking

- Teamwork.



Learning outcomes:

R1. To write, in an orderly manner, and using correct scientific language, the stages of the general analysis process applied to different cases related to pharmaceutical field.

R2. To present solved numerical problems related to the calculation of the concentrations of the different species in equilibrium in acid-base, complex formation, precipitation and oxidation-reduction systems.

R3. To present hand-drawn logarithmic concentration diagrams on graph paper. Students must also attach a written interpretation to the different types of logarithmic diagrams to deduce the concentrations of the different species in a system at equilibrium.

R4. To design or select and apply classic analysis techniques, volumetry and gravimetry, to solve specific problems within the pharmaceutical field.

R5. To write in an orderly manner and using appropriate scientific language, sampling plans for samples of solid and liquid nature.

R6. To describe the preparation process for solid and liquid samples. Likewise, students must select among the procedures of the preparation stage, those most appropriate for each type of sample.

R7. To describe the basic operation of analytical chromatographic instruments, as well as the analytical measurement process.

R8. To carry out chemical analysis of drug samples in the laboratory, interpreting the obtained results.

R9. To correctly solve numerical problems related to the calculation of the analyte concentration in different matrices based on different quantification methods.

R10. To design and execute laboratory practices in accordance with Good Environmental Practices.

BLOCK I. INTRODUCTION.



TOPIC 1.THE GLOBAL ANALYTICAL PROCESS

Concepts of Analytical Chemistry and Chemical Analysis. Terms in Analytical Chemistry. Analytical Chemistry as a science of chemical information. The analytical problem. Stages involved in solving an analytical problem. Importance and evaluation of the quality of analytical results.

TOPIC 2. SELECTION OF THE ANALYSIS METHOD

Factors to consider when selecting the analysis method: Types of methods. Quality parameters of an analytical method. Calibration. Validation of an analytical method.

TOPIC 3. SAMPLING

Introduction. Definition of terms. Sample types. Types of sampling. Representativeness of sampling. Sampling plan. General sampling strategies. Sampling procedures for solids, liquids and gases. Transport and conservation of the sample Examples.

TOPIC 4. PRETREATMENT OF THE SAMPLE

Introduction. Sample preparation for organic and inorganic analysis. Solid-liquid extraction.



BLOCK II. GLOBALISED TREATMENT OF CHEMICAL EQUILIBRIA IN SOLUTION AND ITS APPLICATIONS.

TOPIC 5.ACID-BASE BALANCE.

Exact and approximate calculation of the acidity of different types of solutions. Logarithmic concentration diagrams. Species distribution diagram. Treatment of mixtures. Analytical applications: Acid-base volumetrics.

TOPIC 6. BALANCE OF COMPLEX FORMATION.

Complex species concept. Global and successive training constants. Calculation of concentrations at equilibrium. Logarithmic and predominance area diagrams. Parasitic reactions: graphic treatment. Applications: Complex formation volumetrics.

TOPIC 7. PRECIPITATION BALANCE.

Generalities. Solubility and solubility product. Factors affecting the value of the solubility product. Factors affecting the value of the ionic product. Diagrams of heterogeneous systems. Predominance area diagrams. Fractional precipitation. Competitive reactions. Conditional solubility product. Calculation of concentrations at equilibrium. Applications: Precipitation volumetrics. Gravimetric analysis.

TOPIC 8.OXIDATION-REDUCTION BALANCE.

Equilibrium constant and chemical potential. Calculation of concentrations at equilibrium. Factors that modify the redox potential. Conditional potentials. Predominance area diagrams. Dismutation and stabilization of oxidation degrees. Graphic treatment. Applications: Redox volumetrics, volumetric methods of organic analysis.



BLOCK III.ANALYTICAL SEPARATION TECHNIQUES

TOPIC 9. EXTRACTION AND CLEAN-UP TECHNIQUES

Liquid-liquid extraction. Equilibrium and basic principles. Factors that modify the extraction equilibrium. Solvent selection criteria. Solid phase extraction. Foundation of the process. Factors that affect process performance. Solid phase microextraction. Applications to real samples.

TOPIC 10. CHROMATOGRAPHIC TECHNIQUES

Fundamentals of chromatographic separation. Classification of chromatographic techniques. Types of interaction. Qualitative and quantitative analysis.

TOPIC 11.GAS CHROMATOGRAPHY

Introduction. Carrier gas. Injectors and sampling systems. Chromatographic columns. Detection systems. Applications.

TOPIC 12.LIQUID CHROMATOGRAPHY

Introduction. Classification. Basic components of a liquid chromatography system. Applications.



LABORATORY PRACTICES:

PRACTICE 1. ACID-BASE VOLUMETRY

PRACTICE 2. COMPLEX FORMATION VOLUMETRIES. COMPLEXOMETRIES

PRACTICE 3. OXIDATION-REDUCTION VOLUMETRY

PRACTICE 4. Determination of calcium in pharmaceutical formulations by atomic absorption spectrophotometry.

PRACTICE 5. Determination of the iron content in an antianemic by molecular absorption spectrophotometry in the visible range.

PRACTICE 6. Determination of fluoride in a mouthwash using direct potentiometry with an ion-selective electrode.

The main objective of Analytical Chemistry in the Degree in Pharmacy is the theoretical and practical resolution of analytical problems related to the pharmaceutical field. To do this, students must know all the stages of the general analysis process, which are presented and addressed in the classroom and in the laboratory, combining traditional methodology and problem-based learning. Throughout the entire subject, students must do different types of individual and group tasks and once the proposed learning objectives have been acquired, they must be able to apply them to solve a series of analytical problems, which will be revised by the lecturer giving the corresponding feedback. To facilitate these tasks, master classes will be given on the most relevant content, and questions and debates will be raised in the classroom to encourage student participation. In addition, a series of experimental works will be carried out that will allow the knowledge acquired to be integrated and the skills necessary for work in the laboratory to be developed. Throughout these laboratory practices, students must solve a series of analytical problems in groups using the Inquiry-Based Learning methodology. To do this, they must search, select and interpret information from different sources to finally propose a resolution to the problem posed. Likewise, students will be provided with basic notions about Good Environmental Practices in order to promote their responsibility with sustainable development.

• Continuous Assessment System
• Final Assessment System
• Tools and qualification percentages:
  • Written test to be taken (%): 65
  • Realization of Practical Work (exercises, cases or problems) (%): 25
  • Team projects (problem solving, project design)) (%): 10

Continuous evaluation system:



1. Evaluation of laboratory practices (25% of the overall grade):

* (a) Completion of the practices and practical exam in the laboratory: 10%

* (b) Written test concerning laboratory practices: 15%



The competences of degree 1,2, 3, and 4 and the specific competencies of the subject A1, A3, A4, A7, A9 and A10 will be evaluated. To apply the 25% weighting in the overall grade of the subject, it will be necessary to obtain a 5 out of 10 in each of the sections (a and b) mentioned above. If not, the practices will not be considered passed and, therefore, neither will the subject.



2. Collaborative activities. Resolution of practical cases: 10% of the overall grade. These activities will allow the evaluation of the competencies of Grade 2 and 3 and those specific to the subject A1, A4, A5, A6, A7, A8 and A10.



3. Individual written tests: 65% of the overall grade for the subject.

Several individual written tests will be carried out throughout the quarter, the characteristics of which will be detailed in the students' notebook. One of them will consist of an individual final test where all the knowledge and skills of the subject will be evaluated. This test will consist of two different parts: a first part corresponding to Block II of the syllabus and a second part corresponding to blocks I and III and will include different calculation problems and theory questions. The grade for this test will be obtained from the average of the grades obtained in each individual part. To pass this individual test it is necessary to obtain a score of 5 out of 10 in each of the two parts of the final test. The subject cannot be passed without having passed the final individual test. Competencies between A1 and A8 will be evaluated. To carry out these tests, students must have their own scientific calculator.



The evaluation criteria will be attached in more detail through rubrics in the student guide.



Final evaluation system:

In accordance with the Regulations governing the Evaluation of students in official Degree Degrees (Agreement of the Governing Council of the UPV/EHU of December 15, 2016, published in the BOPV on March 13, 2017), students will have right to be evaluated through the final evaluation system. For this, they must submit in writing to the teaching staff responsible for the subject the waiver to continuous evaluation within a period of 9 weeks from the beginning of the quarter, in accordance with the academic calendar from the centre. These students must prove the acquisition of the skills through a final evaluation that will consist of one or several tests concerning all the topics and concepts worked on the entire subject, both practical and theoretical.



Waiver:

Based on the provisions of the agreement of May 30, 2019, of the Governing Council of the University of the Basque Country / Euskal Herriko Unibertsitatea, which approves the modification of article 12.2 of the Regulations Regulating Student Evaluation in the official Degree qualifications (https://www.euskadi.eus/y22-bopv/es/bopv2/datos/2019/06/1903193a.pdf), given that the weight of the final test for the continuous evaluation system is greater than 40%, not taking the final evaluation test will mean automatic waiver to the corresponding call, both for the continuous evaluation system and for the final evaluation system. Waiver to the call will result in the qualification of not presented.



Continued neglect of spelling and grammar rules in the different tests, exercises or assignments carried out for evaluation may result in a penalty in your grade. This criterion will be applied regardless of the continuous or final evaluation system.

In the extraordinary call, a final test will be carried out including all the theoretical and practical contents of the subject, which will allow the evaluation of all the competences detailed above. Failure to take the final test will result in automatic waiver of the call.

Lab coat, safety glasses, permanent marker, scientific calculator, laboratory notebook.

Basic bibliography

-SKOOG, D. A., HOLLER, F. J. y CROUCH, S. R. Principios de Análisis Instrumental. 6ª ed. Madrid: Paraninfo, 2008.

-HARRIS, D. C. Análisis Químico Cuantitativo. 3ª ed. Barcelona: Reverté, 2006.

-SKOOG, D. A., WEST, D. M., HOLL, F. J., y CROUC, S. R. Fundamentos de Química Analítica. 8ª ed. México: Thomson, 2005.

-ROUESSAC, F. y ROUESSAC, A. Análisis Químico. Métodos y Técnicas Instrumentales Modernas. 1ª ed. Madrid: McGraw-Hill, 2003.

-HARVEY, D. Química Analítica Moderna. 1ª ed. Madrid: McGraw-Hill-Interamericana, 2002.

-HERNÁNDEZ, L. H. y GONZÁLEZ, C. Introducción al Análisis Instrumental. 1ª ed. Barcelona: Ariel, 2002.

-RUBINSON, K. A. y RUBINSON, J. F. Análisis Instrumental. 1ª ed. Madrid: Pearson Educación, 2001.

In-depth bibliography

BLOCK 1
-CÁMARA, C. y HERNANDO, P. F. Toma y Tratamiento de Muestras. 1ª ed. Madrid: Síntesis, 2004.
-CHAN, C. C., LEE, Y. C., LAM, H. and ZHANG, X. M. Analytical Method Validation and Instrument Performance Verification. 1ª ed. Hoboken: Wiley, 2004.
-MILLER, J. N. y MILLER, J. C. Estadística y Quimiometría para Química Analítica. 4ª ed. Madrid: Pearson Educación, 2002.
-VALCÁRCEL, M. y RÍOS, A. La calidad en los laboratorios analíticos. 1ª ed. Barcelona: Reverté, 1992.

BLOCK II
-SÁNCHEZ BATANERO, P. y GÓMEZ DEL RÍO, M. I. Química Analítica General: Equilibrios en Disolución y Métodos Analíticos. 1ª ed. Madrid, 2006.
-BURRIEL MARTÍ, F., LUCENA CONDE, Y., ARRIBAS JIMENO, S. y HERNÁNDEZ MÉNDEZ, J. Química analítica Cualitativa. 18ª ed. Madrid: Paraninfo, 2002.
-SILVA, M. y BARBOSA, J. Equilibrios Iónicos y sus Aplicaciones Analíticas. 1ª ed. Madrid: Síntesis, 2002.
-AGUILAR, M. Introducción a los Equilibrios Iónicos. 2ª ed. Barcelona: Reverté, 1998.

BLOCK III
-CÁMARA, C. y PÉREZ, C. Análisis Químico de Trazas. 1ª ed. Madrid: Síntesis, 2011.
-PAWLISZYN, J. and LORD, H. L. Handbook of Sample Preparation. 1ª ed. Ontario: John Wiley & Sons, 2010.
-CELA, R., LORENZO, R. A. y CASAIS, M. C. Técnicas de Separación en Química Analítica. 1ª ed. Madrid: Síntesis, 2003.
-MITRA, S. Sample Preparation Techniques in Analytical Chemistry. 1ª ed. Hoboken: John Wiley & Sons, 2003.

BLOCK IV
-POLO, L. M. Fundamentos de Cromatografía. 1ª ed. Madrid: Dextra, 2015.
-KAZAKEVICH, Y. V. and LOBRUTTO, R. HPLC for Pharmaceutical Scientists. 1ª ed. Hoboken: Wiley, 2007.
-DONG, M. W. Modern HPLC for Practicing Scientists. 1ª ed. Hoboken: Wiley, 2006.
-MILLER, J. M. Chromatography: Concepts and Contrasts. 2ª ed. Hoboken: Wiley, 2005
-CAZES, J. and SCOTT, R. P. W. Chromatography Theory. 1ª ed. New York: Marcel Dekker, 2002.
-BRAITHWAITE, A. and SMITH, J. F. Chromatographic Methods. 5ª ed. Amsterdam: Springer, 1999

Journals

TrAC, Trends in Analytical Chemistry
https://www.sciencedirect.com/journal/trac-trends-in-analytical-chemistry

Analytical Chemistry
https://pubs.acs.org/journal/ancham

Analyst
https://www.rsc.org/journals-books-databases/about-journals/analyst?gad_source=1&gclid=EAIaIQobChMI-aj7nbKShgMVk0FBAh1xIw1bEAAYASAAEgLemvD_BwE

Web addresses

Compendio de Terminología Química de la IUPAC. (consulta junio de 2040). Disponible en: http://goldbook.iupac.org/

Analytical Chemistry 2.1. David Harvey. (consulta junio de 2024). Texto en línea de libre acceso. Disponible en: https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Analytical_Chemistry_2.1_(Harvey)

Chromacademy. (consulta junio de 2024). Disponible en: http://www.chromacademy.com/

Graphpad. (consulta junio de 2024). Disponible en: http://www.graphpad.com/quickcalcs/contMenu/

Chemical equilibrium diagrams. (consulta junio de 2024). Disponible en: https://sites.google.com/site/chemdiagr/home

EHUagenda 2030 por el desarrollo sostenible. (consulta junio de 2024). Disponible en: https://www.ehu.eus/es/web/iraunkortasuna/ehuagenda-2030