The document discusses the development and validation of an LC-MS/MS bioanalytical method for the determination of a drug in human plasma. It describes the objectives, which are to develop a specific, reliable and cost-effective method. It outlines the key steps in method development including literature search, reference standard preparation, extraction procedure selection, and optimization of separation and detection. The validation parameters that will be evaluated are also summarized, including specificity, accuracy, precision, recovery, matrix effects and stability.
Analytical method validation as per ich and usp shreyas B R
Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Analytical method validation as per ich and usp shreyas B R
Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Bioanalytical Method Development and Validation..
Bioanalytical method validation include all the procedure that demonstrate that a particular method used for quantitative measurement of analyte in given biological matrix are reliable and reproducible for intended use.
Analytical method validation, ICH Q2 guidelineAbhishek Soni
Analytical Method Validation, ICH Q2 Guideline.
General principles related to the analytical method validation.
Validation of analytical method as per International Council for Harmonisation(ICH) guidelines and the United States Pharmacopeia(USP).
Glossary.
Useful in understanding the terms :
Specificity
Linearity
Range
Accuracy
Precision
Detection limit
Quantitation limit
Robustness
Ruggedness
System suitability testing
Ion pair chromatography for pharmacy studentsabhishek rai
Ion-PairChromatography
A GENERALISED OVERVIEW
Chromatography
HPLC
Reverse Phase Chromatography
Ion Pair Chromatography
Ion Pair Reagent
Mechanism of Ion Pair Chromatography
Ion Pair Wash Procedure
Validation of Analytical and Bioanalytical methodssarikakkadam
Guidelines for Validation of Analytical and Bioanalytical methods as per ICH (Q2R1) and USFDA respectively with an example of Bioanalytical method validation.
Bioanalytical Method Development and Validation..
Bioanalytical method validation include all the procedure that demonstrate that a particular method used for quantitative measurement of analyte in given biological matrix are reliable and reproducible for intended use.
Analytical method validation, ICH Q2 guidelineAbhishek Soni
Analytical Method Validation, ICH Q2 Guideline.
General principles related to the analytical method validation.
Validation of analytical method as per International Council for Harmonisation(ICH) guidelines and the United States Pharmacopeia(USP).
Glossary.
Useful in understanding the terms :
Specificity
Linearity
Range
Accuracy
Precision
Detection limit
Quantitation limit
Robustness
Ruggedness
System suitability testing
Ion pair chromatography for pharmacy studentsabhishek rai
Ion-PairChromatography
A GENERALISED OVERVIEW
Chromatography
HPLC
Reverse Phase Chromatography
Ion Pair Chromatography
Ion Pair Reagent
Mechanism of Ion Pair Chromatography
Ion Pair Wash Procedure
Validation of Analytical and Bioanalytical methodssarikakkadam
Guidelines for Validation of Analytical and Bioanalytical methods as per ICH (Q2R1) and USFDA respectively with an example of Bioanalytical method validation.
Analytical Method Validation is a process that is used to demonstrate the suitability of an analytical method for an intended purpose.Regulations and quality standards that have an impact on analytical laboratories require analytical methods to be validated.
Method validation is the process of documenting / proving that an analytical method provides analytical data acceptable for the intended use. A pharmaceutical drug product must meet all its specifications throughout its entire shelf-life. The performance of product characteristics throughout the shelf-life must be tested by analytical method for the product’s chemical, physiochemical, microbiological and biological characteristics. The method of analysis used must be validated. This is required to ensure the product’s safety and efficacy throughout all phases of its shelf-life. Validation is the process of establishing documentary evidence demonstrating that a procedure, process, or activity carried out in testing and then production maintains the desired level of compliance at all stages.
A Review on Step-by-Step Analytical Method Validationiosrphr_editor
When analytical method is utilized to generate results about the characteristics of drug related samples it is essential that the results are trustworthy. They may be utilized as the basis for decisions relating to administering the drug to patients. Analytical method validation required during drug development and manufacturing and these analytical methods are fit for their intended purpose. To comply with the requirements of GMP pharmaceutical industries should have an overall validation policy which documents how validation will be performed. The purpose of this validation is to show that processes involved in the development and manufacture of drug, production and analytical testing can be performed in an effective and reproducible manner. This review article provides guidance on how to perform validation characteristics for the analytical method which are utilized in pharmaceutical analysis.
Review on Bioanalytical Method Development in Human Plasmaijtsrd
Bioanalytical methods are widely used to quantitate drugs and their metabolites in plasma matrices and this method are applied to study in the areas of human clinical and nonhuman study. Bioanalytical methods employed for the quantitative estimation of drugs and their metabolites plays an important role in estimation and interpretation of bioequivalence, pharmacokinetic, and toxicokinetic studies. The major bioanalytical role is method development, method validation, and sample analysis. Techniques such as high pressure liquid chromatography HPLC and liquid chromatography coupled with double mass spectrometry LCMS MS can be used for bioanalytical studies. Mayuri Gavhane | Dr. Ravindra Patil | Tejaswini Kande "Review on Bioanalytical Method Development in Human Plasma" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-6 | Issue-7 , December 2022, URL: https://www.ijtsrd.com/papers/ijtsrd52578.pdf Paper URL: https://www.ijtsrd.com/chemistry/analytical-chemistry/52578/review-on-bioanalytical-method-development-in-human-plasma/mayuri-gavhane
5-Scientific Approach to Validation.pptxAllanThomas30
Validation is a Science and even the most mundane tasks in healthcare environments, like hand washing, must be validated (to ensure correct method and other factors like correct hand wash agent) and also verified - to create an acceptable baseline for post handwash counts.
An Analysis on the UV-Visible Spectrophotometry MethodAI Publications
In the pharmaceutical industry, quality control is a necessary process. Pharmaceutical medicinal products must be advertised as safe, therapeutically active formulations with predictable qualities and performance. The main aim of the study is an analysis on the UV-Visible Spectrophotometry Method. UV spectroscopy was performed on Shimadzu 1700 uv spectrometer, 1cm cell quartz cuvette. Mode was set as UV mode and Detector wavelength was kept at 231 nm and 276 nm. A simple, rapid, accurate, sensitive and cost economical methodology for simultaneous estimation and precise ultraviolet radiation methodology has been developed and valid as per ICH guidelines for simultaneous Estimation of MET and AGP in Their Combined dose form.
General Principles of Analytical Method of Validation.pdfTamannaKumari8
Validation is the process of establishing documentary evidence demonstrating that a procedure, process, activity carried out in
testing and then production maintain the desirable level of compliance all stages.
The process of providing the analytical procedure is acceptable or its intended us.(ICH Q
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Microteaching is a unique model of practice teaching. It is a viable instrument for the. desired change in the teaching behavior or the behavior potential which, in specified types of real. classroom situations, tends to facilitate the achievement of specified types of objectives.
Title: Sense of Smell
Presenter: Dr. Faiza, Assistant Professor of Physiology
Qualifications:
MBBS (Best Graduate, AIMC Lahore)
FCPS Physiology
ICMT, CHPE, DHPE (STMU)
MPH (GC University, Faisalabad)
MBA (Virtual University of Pakistan)
Learning Objectives:
Describe the primary categories of smells and the concept of odor blindness.
Explain the structure and location of the olfactory membrane and mucosa, including the types and roles of cells involved in olfaction.
Describe the pathway and mechanisms of olfactory signal transmission from the olfactory receptors to the brain.
Illustrate the biochemical cascade triggered by odorant binding to olfactory receptors, including the role of G-proteins and second messengers in generating an action potential.
Identify different types of olfactory disorders such as anosmia, hyposmia, hyperosmia, and dysosmia, including their potential causes.
Key Topics:
Olfactory Genes:
3% of the human genome accounts for olfactory genes.
400 genes for odorant receptors.
Olfactory Membrane:
Located in the superior part of the nasal cavity.
Medially: Folds downward along the superior septum.
Laterally: Folds over the superior turbinate and upper surface of the middle turbinate.
Total surface area: 5-10 square centimeters.
Olfactory Mucosa:
Olfactory Cells: Bipolar nerve cells derived from the CNS (100 million), with 4-25 olfactory cilia per cell.
Sustentacular Cells: Produce mucus and maintain ionic and molecular environment.
Basal Cells: Replace worn-out olfactory cells with an average lifespan of 1-2 months.
Bowman’s Gland: Secretes mucus.
Stimulation of Olfactory Cells:
Odorant dissolves in mucus and attaches to receptors on olfactory cilia.
Involves a cascade effect through G-proteins and second messengers, leading to depolarization and action potential generation in the olfactory nerve.
Quality of a Good Odorant:
Small (3-20 Carbon atoms), volatile, water-soluble, and lipid-soluble.
Facilitated by odorant-binding proteins in mucus.
Membrane Potential and Action Potential:
Resting membrane potential: -55mV.
Action potential frequency in the olfactory nerve increases with odorant strength.
Adaptation Towards the Sense of Smell:
Rapid adaptation within the first second, with further slow adaptation.
Psychological adaptation greater than receptor adaptation, involving feedback inhibition from the central nervous system.
Primary Sensations of Smell:
Camphoraceous, Musky, Floral, Pepperminty, Ethereal, Pungent, Putrid.
Odor Detection Threshold:
Examples: Hydrogen sulfide (0.0005 ppm), Methyl-mercaptan (0.002 ppm).
Some toxic substances are odorless at lethal concentrations.
Characteristics of Smell:
Odor blindness for single substances due to lack of appropriate receptor protein.
Behavioral and emotional influences of smell.
Transmission of Olfactory Signals:
From olfactory cells to glomeruli in the olfactory bulb, involving lateral inhibition.
Primitive, less old, and new olfactory systems with different path
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Anti-ulcer drugs are medications used to prevent and treat ulcers in the stomach and upper part of the small intestine (duodenal ulcers). These ulcers are often caused by an imbalance between stomach acid and the mucosal lining, which protects the stomach lining.
||Scope: Overview of various classes of anti-ulcer drugs, their mechanisms of action, indications, side effects, and clinical considerations.
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2. Introduction
Objective
Method Development
Method Validation
Validation Parameter
Plan of Work
Reference
22
3. Bioanalytical Method relates specifically to determine the
concentration of drug or its metabolite or both in biological
matrix such as plasma, serum, urine , etc
Bioanalytical information used in human clinical
pharmacology, bioavailablity (BA) and bioequivalence (BE)
studies requiring pharmacokinetic evaluation
Bioanalytical method is also used for non human
pharmacology/ toxicology studies (preclinical studies)
4. LC/MS/MS is a hyphenated technique that combines
physical separation power of liquid chromatography
with detection power of Mass spectrometry.
LC/MS/MS is a powerful technique used for many
application which have very high sensitivity and
specificity
44
5. • To develop and validate highly specific, reliable and cost
effective LC-MS/MS method for determination of drug
in human plasma
• The scope of developing and validating the bioanalytical
method is to get a suitable method which is more
accurate and precise for the analyte of interest under
given set of lab condition by using resources available
55
6. 66
Steps In Method Development
Literature search for drugs.
Identification of analytical techniques and optimization
Reference standard preparation.
Selection of internal standard
Sample pre- treatment (Extraction procedure)
Sample storage
8. Mode of separation
Selection of column
Selection of mobile phase
Role of pH, Buffer
Role of Temperature
Role of flow rate
88
9. Liquid-Liquid Extraction
Solid phase Extraction
Reduced organic solvent consumption
Easier collection of the total analyte fraction
More efficient separation of interferences
Protein precipitation
99
10. 1100
Validation
What is Validation and why should it be done ?
Validation is the process of determining the suitability
of a
given methodology for providing useful analytical data
Validation is required for any new method to ensure that it
is capable to give reproducible and reliable results, when
used by different operators employing the same
equipment in the same or different laboratories
11. 1111
Definition of Bioanalytical Method
Validation
Bioanalytical method validation include all the procedure that
demonstrate that a particular method used for quantitative
measurement of analyte in given biological matrix are reliable
and reproducible for intended use
Types of Method validation
13. Ability of an analytical method to differentiate and
quantify the analyte in the presence of other
components in the sample
Selectivity is evaluated by injecting extracted
blank plasma and comparing with the response of
extracted LLOQ samples processed with internal
standard.
1133
14. Accuracy
Closeness of determined value to the true
value.
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15. The closeness of replicate determinations of a sample by an
assay.
The acceptance criteria is £ 15% CV.
At LOQ, 20% deviation is acceptable.
% CV (precision) =100 x Standard deviation/Mean
It Includes
Repeatability
Intermediate Precision
Reproducibility
16. The detector response obtained from an amount of the
analyte added to and extracted from the biological
matrix, compared to the detector response obtained for
the true concentration of the pure authentic standard.
Recovery pertains to the extraction efficiency of an
analytical method within the limits of variability
1166
17. The effect on an bio-analytical method caused by all
other components of the sample except the specific
compound to be quantified.
The difference in response between a neat sample
solution and the post-extraction spiked sample is called
the absolute matrix effect.
1177
18. Due to ion suppression/enhancement by the others ions
present in the biological matrix which might get
ionized during detection and will give false results.
Matrix effect studied by comparing the response of
extracted samples spiked before extraction with
response of the blank matrix sample to which analyte
has been added at the same nominal concentration just
before injection
1188
19. 1199
chemical stability of an analyte in a given matrix
under specific conditions for given time intervals.
Analyte change in any respect affect the
chromatographic behavior which may complicate the
method development the following activities should be
considered:
•Analyte and IS stock stability in solvent
•Short Term Stability in matrix
•Bench top stability in matrix
•Freeze-thaw stability in matrix
•In-injector stability in matrix
•Long-term stability in matrix
20. literature survey
Selection of analytical technique.
Method Development
Method Validation
Compilation of data
Result & conclusion
2200
21. Food and Drug Administration, FDA, Guidance for Industry: Bioanalytical Method
Validation, Rockville, MD: US Department of Health and Human Services, Food and Drug
Administration, Center for Drug Evaluation and Research, 2013.
Peters F.T., Review: Bioanalytical method validation – How, how much and why, Department
of Experimental and Clinical Toxicology, Institute of Experimental and Clinical
Pharmacology and Toxicology, University of Saarland.
Pranay W, Bioanalytical Method Development –Determination of Drugs in Biological Fluids
2010.
Skoog DA, West DM, Holler FJ, Crouch SR. Fundamentals of Analytical chemistry. 18th ed.
Thomson Asia pvt Ltd. Chapter 1. The nature of analytical chemistry. 2004; 2-5 & 973-996.
Chatwal R. G., Anand K. S. Instrumental method of chemical analysis, Himalaya Publishing
House , Mumbai, 2007, 3rd edition, pp. 2.566 – 2.587, 2.624 – 2.639, 2.272- 2.302.
ICH, Validation of analytical procedure, International conference on Harmonization, IFPMA,
Q2B Validation of Analytical Procedures: Methodology
2211