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أ.د. هيثم بن خالد الربيعة

Professor

قسم الكيمياء الصيدلية

كلية الصيدلة
كلية الصيدلة(مبنى رقم 23) الدور الثاني مكتب رقم 2أ 121
مادة دراسية

(PHC 427 (Pharmaceutical Instrumental Analysis

Course Description:

The course is designed to give pharmacy schools an overview of the various modern instrumental analytical techniques used in the pharmaceutical research and industry. Basic principles, components, and operation of each technique will be presented in an integrative lecture and laboratory sessions.

وصف المقرر:
يختص هذا المقرر بالتحليل الآلي للمركبات الصيدلية. يشمل المقرر الطرق المختلفة للتحليل الآلي. يقدم المقرر بشكل تكاملي بين الدروس النظرية و المعملية التطبيقية لدراسة كل طريقة من طرق التحليل من حيث المفاهيم الأساسية للتحليل والتعريف بمكونات جهاز التحليل ووظيفة كل مكون, وطريقة العمل على جهاز التحليل و استخداماته في المجالات المختلفة من التحليل الصيدلي. 
 (توزيع المنهج) LECTURES’ OUTLINE
 

Week Lecture
number
Date Topic
1 1   Atomic absorption and emission spectrophotometry
Principles of atomic absorption spectrophotometry
2    Factors affecting atomic absorption
3   Instrumentation of atomic absorption spectrophotometry
2 4   Applications of atomic absorption spectrophotometry
5   Principles of atomic emission spectrophotometry
6   Instrumentation of atomic emission spectrophotometry.
3 7   Applications of atomic emission spectrophotometry
8   Optical methods
Polarization of light, theory and instrumentation of polarimetric analysis.
9   Applications of polarimetry in pharmaceutical analysis
4 10   Theory and instrumentation of refractometric analysis.
11   Applications of refractometry
12   Molecular emission spectrophotometry
Theory of light emission
5 13   Fluorescence and phosphorescence
14   Chemical structure and fluorescence
15   Instrumentation of fluorometry
6 16   Applications of fluorometry in direct analysis of fluorescent compounds 
17   Applications of fluorimetry in non-fluorescent compounds after their derivatization
18   Immunoanalytical methods
Principles of immunoassay
7 19   Immunoanalytical reagents
20   Separation matrices in immuoassays
21   Designs, formats, and types of immunoassays
8 22   Detection systems used in immunoassays
23   Instrumentation of immunoassay.
24   Specific features of quantitative analysis by immunoasay.
9 25   Applications of immunoassays, competitive assay
26   Applications of immunoassays, non-competitive assay
27   High performance liquid chromatography  (HPLC):  
Instrumentation of HPLC

    

Week Lecture
number
Date Topic
10 28   Choice of detectors for different groups of drugs
29   Choice of optimum systems for selected groups of drugs
30   Detection of degradation products and exipients
11 31   Chiral separation of pharmaceutical compounds
32   Separation and quantification of mixtures in dosage forms
33   External and internal standard method for quantitative analysis by HPLC
12 34   Stability-indicating Methods of assay
35   Gas Chromatographic
The thermodynamic of gas chromatography.
36   The dynamics of gas chromatography.
13 37   Instrumentation of gas chromatography.
38   Application of gas chromatography
39   Capillary electrophoresis
Principles and instrumentation of capillary electrophoresis
14 40   Choice of optimum conditions for electrophoretic resolution.
41   Modes of electrophoretic separation of compounds.
42   Applications of capillary electrophoresis in pharmaceutical analysis

 

Text books:

 1.Analytical Chemistry. Gary D. Christian. John Wiley & Sons, New York

           2.  Pharmaceutical analysis: a textbook for pharmacy students and pharmaceutical chemists. D. G. Watson. Churchill Livingstone. Edinburgh

Common questions:

Exam 1 (OUT of 10)

Q1: Ethanol and methanol are separated in a capillary column with retention times of  370 and 385 s, respectively, and base widths (Wb) of 16.0 and 17.0 s. An un-retained air peak occurs at 10 s. From these information, calculate:
                                                                                                                                                    ( each worth 1 point)

1. The separation factor (selectivity)? α= (380-10)/(370-10)= 1.04

 

2. The retention factor of each compound?          k1= (370-10)/10=36
         k2= (385-10)/10= 38.5

3. resolution?  Rs= 2(380-370)/(17+16)= 0.91

Q2: Choose the correct question:                                                                                         ( each worth 1 point)                                         

1- In isocratic elution the composition is :

  1. Constant. 
  2. Changed continuously over a period of time.
  3. Changed after predetermined period of time.
  4. All of the above.
  5. None of the above.

The Answer is (A)

 

2- In comparison with HPLC system, UHPLC has_______ pressure pump and ________ particle size

  1. Lower, smaller
  2. Lower, larger
  3. Higher, smaller
  4. Higher, larger

The Answer is (C)

 

3- Sonication is an approach that can act as a             for solvents used in HPLC systems.

  1.  Degasser 
  2. Filtration system
  3. Non-polar column
  4. None of the above

 The Answer is (A)

 

4- For solvent degassing, argon is not a good substitute of helium because it is            : 

  1.  Expensive
  2. Soluble in most liquid
  3. Cheap
  4. Not soluble in most liquid

The answer is (B)

Q3: The fundamental resolution equation indicates that resolution is affected by three important parameters, name these parameters:                                                                                                               (each worth 1 point)

1- Efficiency
2- Retention factor
3- Selectivity

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