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.
Analytical method development and validation for simultaneous estimationProfessor Beubenz
Brief about analytical method development and validation
Subscribe to the YouTube Channel #Professor_Beubenz
https://www.youtube.com/channel/UC84jGf2iRN5VjwnQqi6qmXg?view_as=subscriber
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.
Analytical method development and validation for simultaneous estimationProfessor Beubenz
Brief about analytical method development and validation
Subscribe to the YouTube Channel #Professor_Beubenz
https://www.youtube.com/channel/UC84jGf2iRN5VjwnQqi6qmXg?view_as=subscriber
In this slide contains types of HPLC Columns, Plate theory and Van Deemter Equation.
Presented by : Malarvannan.M (Department of pharmaceutical analysis).
RIPER,anantpur.
Differential spectrophotometric method for estimation and validation of Verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, beeers law limits 525µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamine in simple, precise and economically and it recommended for the routine drug quality analysis investigation.
In this slide contains types of HPLC Columns, Plate theory and Van Deemter Equation.
Presented by : Malarvannan.M (Department of pharmaceutical analysis).
RIPER,anantpur.
Differential spectrophotometric method for estimation and validation of Verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, beeers law limits 525µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamine in simple, precise and economically and it recommended for the routine drug quality analysis investigation.
Differential spectrophotometric method for estimation and validation of Verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, beeers law limits 525µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamine in simple, precise and economically and it recommended for the routine drug quality analysis investigation.
Multiple Method Development and Validation for Simultaneous Estimation of Chl...ijtsrd
A simple, precise and accurate multiple analytical method has been developed for the simultaneous estimation of Chlorzoxazone and Nimesulide in bulk and tablet formulations by reversed-phase liquid chromatographic and UV-Visible spectrophotometric techniques. The chromatographic separation was achieved on C18 analytical column. A mixture of Methanol 0.1 Ortho-phosphoric acid 75 25 was used as mobile phase, at a flow rate of 1mL min and detection wavelength at 295 nm. The retention time of Chlorzoxazone and Nimesulide was found to be 4.69 and 5.45 min respectively. The linear dynamic ranges for HPLC were from 2-10 µg mL and for simultaneous equation method, derivative spectroscopy, Q-ratio Absorbance method, Dual wavelength it was 10-30 µg mL for both Chlorzoxazone and Nimesulide. The percentage recovery obtained for Chlorzoxazone and Nimesulide were 100.93 and 102.19 respectively for RP-HPLC, 9.7 and 100.1 for simultaneous equation method of CZ and NIM respectively, 99.97 and 99.78 for derivative spectroscopy of CZ and NIM respectively, 101.37 and 99.48 for Q-ratio Absorbance method of CZ and NIM respectively, 100.13 and 99.96 for dual wavelength method of CZ and NIM respectively. The validation of the proposed methods were carried out for linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The developed method can be used for routine quality control analysis of titled drugs in combination in tablet formulation. Swetha Yarramsetti | A. Elphine Prabahar | Rama Rao Nadendla "Multiple Method Development and Validation for Simultaneous Estimation of Chlorzoxazone and Nimesulide in Bulk and Pharmaceutical Dosage Form" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-2 , February 2019, URL: https://www.ijtsrd.com/papers/ijtsrd21503.pdf
Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/21503/multiple-method-development-and-validation-for--simultaneous-estimation-of-chlorzoxazone-and--nimesulide-in-bulk-and-pharmaceutical-dosage-form/swetha-yarramsetti
Differential spectrophotometric method for estimation and validation of verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, Beers law limits 5-25µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamil in simple, precise and economically and it recommended for the routine drug quality analysis investigation
UV spectrophotometric method development and validation for quantitative esti...Sagar Savale
UV Spectrophotometric Method Development and Validation for quantitative estimation of Ondansetron
Hydrochloride (HCL). U.V Spectrophotometric method have been widely employed in determination of
individual components in a mixture or fixed dose combination. Our aim is to develop spectroscopic method for
estimation of the Ondansetron HCL in ternary mixture by using U.V spectrophotometry. The method was
validated as per ICH guidelines. The recovery studies confirmed the accuracy and precision of the method. It was
successfully applied for the analysis of the drug in bulk and could be effectively used for the routine analysis.
Chromatography is a technique for separating various inorganic and organic compounds. It is one of the separation techniques used as differential migration. It is more advantageous over conventional separating methods such as crystallization, solvent extraction and distillation. The purpose of presentation is to present various chromatographic techniques included a few advanced forms such as FC, HPLC,UPLC and UPCC (Super Critical chromatography).These are rapid forms of chromatographic techniques based on air pressure driven, optimized for rapid and precise separation of an organic compound.
Development and Validation of Novel RP-HPLC method for the estimation of Nalo...Bhavana Gundavarapu
The RP-HPLC method was developed and validated for quantitative determination of Naloxegol in pharmaceutical dosage forms. The method was validated with regard to linearity, accuracy, precision, selectivity, and robustness. The method was applied successfully for the determination of Naloxegol during kinetic studies in aqueous solutions (pH and thermal degradation).
Development and validation of HPLC method for the estimation of Escitalopram ...SriramNagarajan15
A simple, specific, robust, accurate and precise isocratic HPLC method has been developed and subsequently validated for simultaneous determination of escitalopram (ESP) in pharmaceutical dosage forms. Kromosil (250x4.6)mm 5µ with flow rate of 1ml/ min by using JASCO PU-1580 and UV/VIS JASCO UV-1570 at 238 nm. The separation was carried out using a mobile phase consisting of acetonitrile, methanol and 5mM ammonium acetate buffer (pH 3.0) in the ratio 30:20:50 respectively. The retention time for escitaloparm was found to be 5.36 minutes respectively. The correlation coefficient was found to be 0.9997 (ESP). The mean percentage recovery was found to be 101.86 respectively. The % estimation of the drugs was found near to 100 % representing the accuracy in the method. The proposed method was also validated and applied for the analysis of drugs in tablet formulation.
NVBDCP.pptx Nation vector borne disease control programSapna Thakur
NVBDCP was launched in 2003-2004 . Vector-Borne Disease: Disease that results from an infection transmitted to humans and other animals by blood-feeding arthropods, such as mosquitoes, ticks, and fleas. Examples of vector-borne diseases include Dengue fever, West Nile Virus, Lyme disease, and malaria.
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
Flu Vaccine Alert in Bangalore Karnatakaaddon Scans
As flu season approaches, health officials in Bangalore, Karnataka, are urging residents to get their flu vaccinations. The seasonal flu, while common, can lead to severe health complications, particularly for vulnerable populations such as young children, the elderly, and those with underlying health conditions.
Dr. Vidisha Kumari, a leading epidemiologist in Bangalore, emphasizes the importance of getting vaccinated. "The flu vaccine is our best defense against the influenza virus. It not only protects individuals but also helps prevent the spread of the virus in our communities," he says.
This year, the flu season is expected to coincide with a potential increase in other respiratory illnesses. The Karnataka Health Department has launched an awareness campaign highlighting the significance of flu vaccinations. They have set up multiple vaccination centers across Bangalore, making it convenient for residents to receive their shots.
To encourage widespread vaccination, the government is also collaborating with local schools, workplaces, and community centers to facilitate vaccination drives. Special attention is being given to ensuring that the vaccine is accessible to all, including marginalized communities who may have limited access to healthcare.
Residents are reminded that the flu vaccine is safe and effective. Common side effects are mild and may include soreness at the injection site, mild fever, or muscle aches. These side effects are generally short-lived and far less severe than the flu itself.
Healthcare providers are also stressing the importance of continuing COVID-19 precautions. Wearing masks, practicing good hand hygiene, and maintaining social distancing are still crucial, especially in crowded places.
Protect yourself and your loved ones by getting vaccinated. Together, we can help keep Bangalore healthy and safe this flu season. For more information on vaccination centers and schedules, residents can visit the Karnataka Health Department’s official website or follow their social media pages.
Stay informed, stay safe, and get your flu shot today!
Lung Cancer: Artificial Intelligence, Synergetics, Complex System Analysis, S...Oleg Kshivets
RESULTS: Overall life span (LS) was 2252.1±1742.5 days and cumulative 5-year survival (5YS) reached 73.2%, 10 years – 64.8%, 20 years – 42.5%. 513 LCP lived more than 5 years (LS=3124.6±1525.6 days), 148 LCP – more than 10 years (LS=5054.4±1504.1 days).199 LCP died because of LC (LS=562.7±374.5 days). 5YS of LCP after bi/lobectomies was significantly superior in comparison with LCP after pneumonectomies (78.1% vs.63.7%, P=0.00001 by log-rank test). AT significantly improved 5YS (66.3% vs. 34.8%) (P=0.00000 by log-rank test) only for LCP with N1-2. Cox modeling displayed that 5YS of LCP significantly depended on: phase transition (PT) early-invasive LC in terms of synergetics, PT N0—N12, cell ratio factors (ratio between cancer cells- CC and blood cells subpopulations), G1-3, histology, glucose, AT, blood cell circuit, prothrombin index, heparin tolerance, recalcification time (P=0.000-0.038). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and PT early-invasive LC (rank=1), PT N0—N12 (rank=2), thrombocytes/CC (3), erythrocytes/CC (4), eosinophils/CC (5), healthy cells/CC (6), lymphocytes/CC (7), segmented neutrophils/CC (8), stick neutrophils/CC (9), monocytes/CC (10); leucocytes/CC (11). Correct prediction of 5YS was 100% by neural networks computing (area under ROC curve=1.0; error=0.0).
CONCLUSIONS: 5YS of LCP after radical procedures significantly depended on: 1) PT early-invasive cancer; 2) PT N0--N12; 3) cell ratio factors; 4) blood cell circuit; 5) biochemical factors; 6) hemostasis system; 7) AT; 8) LC characteristics; 9) LC cell dynamics; 10) surgery type: lobectomy/pneumonectomy; 11) anthropometric data. Optimal diagnosis and treatment strategies for LC are: 1) screening and early detection of LC; 2) availability of experienced thoracic surgeons because of complexity of radical procedures; 3) aggressive en block surgery and adequate lymph node dissection for completeness; 4) precise prediction; 5) adjuvant chemoimmunoradiotherapy for LCP with unfavorable prognosis.
micro teaching on communication m.sc nursing.pdfAnurag Sharma
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.
New Drug Discovery and Development .....NEHA GUPTA
The "New Drug Discovery and Development" process involves the identification, design, testing, and manufacturing of novel pharmaceutical compounds with the aim of introducing new and improved treatments for various medical conditions. This comprehensive endeavor encompasses various stages, including target identification, preclinical studies, clinical trials, regulatory approval, and post-market surveillance. It involves multidisciplinary collaboration among scientists, researchers, clinicians, regulatory experts, and pharmaceutical companies to bring innovative therapies to market and address unmet medical needs.
New Directions in Targeted Therapeutic Approaches for Older Adults With Mantl...i3 Health
i3 Health is pleased to make the speaker slides from this activity available for use as a non-accredited self-study or teaching resource.
This slide deck presented by Dr. Kami Maddocks, Professor-Clinical in the Division of Hematology and
Associate Division Director for Ambulatory Operations
The Ohio State University Comprehensive Cancer Center, will provide insight into new directions in targeted therapeutic approaches for older adults with mantle cell lymphoma.
STATEMENT OF NEED
Mantle cell lymphoma (MCL) is a rare, aggressive B-cell non-Hodgkin lymphoma (NHL) accounting for 5% to 7% of all lymphomas. Its prognosis ranges from indolent disease that does not require treatment for years to very aggressive disease, which is associated with poor survival (Silkenstedt et al, 2021). Typically, MCL is diagnosed at advanced stage and in older patients who cannot tolerate intensive therapy (NCCN, 2022). Although recent advances have slightly increased remission rates, recurrence and relapse remain very common, leading to a median overall survival between 3 and 6 years (LLS, 2021). Though there are several effective options, progress is still needed towards establishing an accepted frontline approach for MCL (Castellino et al, 2022). Treatment selection and management of MCL are complicated by the heterogeneity of prognosis, advanced age and comorbidities of patients, and lack of an established standard approach for treatment, making it vital that clinicians be familiar with the latest research and advances in this area. In this activity chaired by Michael Wang, MD, Professor in the Department of Lymphoma & Myeloma at MD Anderson Cancer Center, expert faculty will discuss prognostic factors informing treatment, the promising results of recent trials in new therapeutic approaches, and the implications of treatment resistance in therapeutic selection for MCL.
Target Audience
Hematology/oncology fellows, attending faculty, and other health care professionals involved in the treatment of patients with mantle cell lymphoma (MCL).
Learning Objectives
1.) Identify clinical and biological prognostic factors that can guide treatment decision making for older adults with MCL
2.) Evaluate emerging data on targeted therapeutic approaches for treatment-naive and relapsed/refractory MCL and their applicability to older adults
3.) Assess mechanisms of resistance to targeted therapies for MCL and their implications for treatment selection
263778731218 Abortion Clinic /Pills In Harare ,sisternakatoto
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MANAGEMENT OF ATRIOVENTRICULAR CONDUCTION BLOCK.pdfJim Jacob Roy
Cardiac conduction defects can occur due to various causes.
Atrioventricular conduction blocks ( AV blocks ) are classified into 3 types.
This document describes the acute management of AV block.
- Video recording of this lecture in English language: https://youtu.be/lK81BzxMqdo
- Video recording of this lecture in Arabic language: https://youtu.be/Ve4P0COk9OI
- Link to download the book free: https://nephrotube.blogspot.com/p/nephrotube-nephrology-books.html
- Link to NephroTube website: www.NephroTube.com
- Link to NephroTube social media accounts: https://nephrotube.blogspot.com/p/join-nephrotube-on-social-media.html
Explore natural remedies for syphilis treatment in Singapore. Discover alternative therapies, herbal remedies, and lifestyle changes that may complement conventional treatments. Learn about holistic approaches to managing syphilis symptoms and supporting overall health.
ARTIFICIAL INTELLIGENCE IN HEALTHCARE.pdfAnujkumaranit
Artificial intelligence (AI) refers to the simulation of human intelligence processes by machines, especially computer systems. It encompasses tasks such as learning, reasoning, problem-solving, perception, and language understanding. AI technologies are revolutionizing various fields, from healthcare to finance, by enabling machines to perform tasks that typically require human intelligence.
1. ANALYTICAL METHOD DEVELOPMENT
1
Mr. Sagar Kishor Savale
[Department of Pharmaceutics]
avengersagar16@gmail.com
2015-2016
Department of Pharmacy (Pharmaceutics) | Sagar savale
4/28/2016 Sagar Savale
2. Need
» Herbal Products
» New process and reactions
» New molecules
» Active ingredients (Macro analysis)
» Residues (Microanalysis)
» Impurity Profiling
» Component of Interest in different matrices
24/28/2016 Sagar Savale
3. Outcomes
Analytical method gives-
» The required data for a given analytical problem
» The required sensitivity
» The required accuracy
» The required range of analysis
» The required precision
34/28/2016 Sagar Savale
4. Basic criteria
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.
44/28/2016 Sagar Savale
6. Spectrophotometric Methods of Analysis For
Drugs In Combination
The basis of all the spectrophotometric techniques for multicomponent
samples is the property that at all wavelengths:
- the absorbance of a solution is the sum of absorbance of the individual
components or
- the measured absorbance is the difference between the total absorbance of
the solution in the sample cell and that of the solution in the reference cell.
64/28/2016 Sagar Savale
7. Nature of analysis
Single component analysis
- Use of standard absorptivity value
- Use of calibration curve
-Single or double point standardization
Multicomponent analysis
-Simultaneous equation method
-Two wavelength method
-The absorption ratio method
-Geometric correction method
-Absorption factor method
-Orthogonal polynomial method
-Difference spectrophotometry
-Derivative spectrophotometry
-Area under curve method
74/28/2016 Sagar Savale
8. Simultaneous Equation Method
Condition-
If a sample contains two absorbing drugs (X &
Y) each of which absorbs at the lambda max of
each other.
Equation -
Cx = (A2 ay1 - A1 ay2) / (ax2 ay1 - axay2)
Cy = (A1 ax2 - A2 ax1) / (ax2 ay1 - ax1ay2)
Where,
ax1 and ax2 - absorptivities of X at λ1 and λ2
respectively
ay1 and ay2 - absorptivities of Y at λ1 and λ2
respectively
A1 and A2 - absorbance of the diluted sample
at λ1 and λ2 respectively.
Cx and Cy be the concentration of X and Y
in the diluted samples respectively
8
Fig.1The overlain spectra of substance X and
Y, showing the wavelength for the assay of X
and Y in admixture by the method of
simultaneous equation.
4/28/2016 Sagar Savale
9. Examples of reported Drugs
- Estimation of Gliclazide and Metformin hydrochloride in
combined dosage forms.
- Estimation of Losartan potassium and Hydrochlorothiazide in
tablets.
- Estimation of Salbutamol and Theophylline from tablets.
- Estimation of Amlodipine besylate and Enalepril maleate from
tablets.
94/28/2016 Sagar Savale
10. Example
Ultraviolet Spectrophotometric determination of Olmesartan medoxomil &
Hydrochlorothiazide in pharmaceutical formulation by simultaneous equation
method
10
Fig.2 Overlay of Olmesartan medoxomil & Hydrochlorothiazide
Fig.3 Overlay of mixed sample of Olmesartan medoxomil & Hydrochlorothiazide
4/28/2016 Sagar Savale
11. Q-Absorbance Method (Absorbance Ratio
Method)
• The ratio of absorbance's at any two
wavelengths is a constant value
independent of concentration or path
length
• For example, two different dilution
of the same substance give the same
absorbance ratio A1/A2.
• In the USP, this ratio is referred to as
Q value
• Absorbance's are measured at two
wavelengths :-
-λmax of one of the component (λ2)
-wavelength of equal absorptivity's
of the two components i.e. an is
absorptive point. 11
Fig. 4 Wavelength for the assay of
substances X and Y in admixture by the
method of absorbance ratio method4/28/2016 Sagar Savale
12. Example
Estimation of Valsartan and Hydrochlorothiazide in pharmaceutical dosage
form by absorption ratio method 7
12
Fig. 5Overlay spectra of Valsartan & Hydrochlorothiazide showing iso-absorptive point at 231.5nm
4/28/2016 Sagar Savale
13. Q-Absorbance Method (Absorbance Ratio
Method)
Examples -
• - Estimation of Rifampicin and Isoniazid in pharmaceutical dosage forms.
• - Estimation of Spironolactone and hydroflumethiazide.
• - Estimation of Nalidixic acid and Metronidazole from tablets.
• - Estimation of Noscapine, Chlorpheniramine Maleate and Ephedrine
hydrochloride from tablets.
134/28/2016 Sagar Savale
14. Derivative Spectroscopy
• Derivative spectrophotometry involves the conversions of a normal
spectrum to its first, second or higher derivative spectrum.
• Advantages -
1.Enhanced resolution
2.Bandwidth discrimination
• Methods of derivative spectroscopy -
1.Modification of the optical system
2.Electronic differentiation of the spectrophotometer analogue signal
3.Microcomputer differentiation
144/28/2016 Sagar Savale
15. Examples of reported drugs
-Estimation of Propranolol and Hydrochlorothiazide.
-Estimation of Phenylpropanolamine, Chlorpheniramine and
Bromhexine.
-Estimation of Naphazoline hydrochloride and Chlorpheniramine
maleate.
154/28/2016 Sagar Savale
16. Derivative Spectroscopy (continue)
Development and validation of spectrophotometric method for simultaneous
estimation of Samaritan and Naproxen sodium in tablet dosage form 8
16
Fig .6 First derivative overlain spectra of SUM and NAP
Solvent : Methanol; Zero crossing point at 298nm & 335nm for SUM & NAP resp.
4/28/2016 Sagar Savale
17. Difference Spectroscopy
17
Fig.7 Difference spectrum of BSZ (10 μg/mL solution of BSZ in 0.1 M HCl was taken
as blank and the same concentration of drug in 0.1 M NaOH as sample).
Abs.
wavelength
4/28/2016 Sagar Savale
18. Multicomponent mode of analysis
18
Fig .8 UV spectrum of Ceftriaxone sodium and
Sulbactam sodium
Fig. 9Assay report of ceftriaxone sodium and
sulbactam sodium by multi-component mode
of analysis
Solvent : 0.1 Sodium Hydroxide ; Wavelenght :251nm(Sulbactum) & 259nm(Ceftriaxone)4/28/2016 Sagar Savale
19. Solvent Extraction Method
• Separation of individual drugs based on their selective solubility
followed by spectrophotometric measurement.
• Separate the absorbing interfering from the analyte by solvent
extraction procedure.
• Examples :-
-Estimation of Probenecid and Ampicillin from tablets.
-Estimation of Probenecid and Cephalexine from tablets.
-Estimation of Caffeine from Aspirin and Caffeine tablets.
-Estimation of Paracetamol and Diclofenac sodium from tablets.
194/28/2016 Sagar Savale
20. Chemical Derivatisation
Indirect spectrophotometric assays
Conversion of the analyte by a chemical reagent to a derivative that has
different spectral properties
Reasons for adopting chemical Derivatisation
1.Weak absorption of the analyte
2.Interference from irrelevant absorption
3.Improve selectivity of the assay
4.Cost
204/28/2016 Sagar Savale
21. Chemical Derivatisation
Methods
1.Diazotisation & coupling of primary aromatic amines
2.Condensation reactions
3.Reduction of tetrazolium salts
4.Acid – dye method
5.Oxidation methods
6.Metal legand complexation
214/28/2016 Sagar Savale
22. Example
Development and validation of spectrophotometric method for estimating
Amisulpride in pharmaceutical preparations11
Diazotisation & coupling of primary aromatic amines
Diazotization of Amisulpride with sodium nitrite and hydrochloric acid,
followed by coupling with -
-N-(1-naphthyl) ethylenediamine hydrochloride (Method A),
-diphenylamine (Method B),
- β-naphthol in an alkaline medium (Method C),
- resorcinol in an alkaline medium (Method D) &
- chromotropic acid in an alkaline medium (Method E) to form a colored
chromogen.
The absorption maxima, λmax, are at
-523 nm for Method A,
-382 and 490 nm for Method B,
-527 nm for Method C,
-521 nm for Method D and
-486 nm for Method E.
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23. Area under curve method
23
Fig.10 Overlay spectrum of RAM and HCT
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24. Analytical method validation
Accuracy
Precision
Linearity
Range
Limit of Quantitation
Limit of Detection
Ruggedness
Robostnes
Specificity
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25. References
1. Rashmin. An Introduction To Analytical Method Development For
Pharmaceutical Formulations .Pharma info.net 2008 July 22;6(4):1-27
2. Sethi PD.Quantitative Analysis of Drugs In Pharmaceutical
Formulations.3rd ed. New Delhi, CBS Publishers & distributors;2005, p.7
3. Saraf S. Various UV spectrophotometric simultaneous estimation
methods.Pharma info.net 2006 April 04;4(2)
4. Daharval SJ.Methods of estimation of multi -component formulations.
Pharma info.net 2006 June 19;4(3)
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