This document discusses the calibration and validation of various analytical instruments used in pharmaceutical analysis. It provides details on calibrating UV-Vis spectrophotometers, IR spectrophotometers, spectrofluorimeters, HPLC, and GC. Calibration ensures instrument readings are accurate against standards, while validation confirms the instrument is correctly installed and operating as intended. The document outlines tests and acceptance criteria for evaluating characteristics like wavelength accuracy, resolution, noise, baseline flatness, sensitivity, flow rate, and linearity during calibration and validation of different analytical instruments.
The objective of any chemical analytical measurement is to get consistent, reliable and accurate data.
Proper functioning and performance of analytical instruments and computer systems plays a major role in achieving this goal.
Therefore, analytical instrument qualification (AIQ) and calibration should be part of any good analytical practice.
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 objective of any chemical analytical measurement is to get consistent, reliable and accurate data.
Proper functioning and performance of analytical instruments and computer systems plays a major role in achieving this goal.
Therefore, analytical instrument qualification (AIQ) and calibration should be part of any good analytical practice.
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.
QUALIFICATION OF UV-VISIBLE SPECTROPHOTOMETER, FTIR, DSC, HPLCAnupriyaNR
Analytical method qualification consists of a simplified evaluation of a subset of validation characteristics with a goal to demonstrate that an analytical method is scientifically sound and suitable for its intended use. In contrast to validation, analytical method qualification is performed without predefined acceptability criteria. Qualification may be performed as a prerequisite to method validation, or when an assay for product knowledge has not yet been established as a test for a critical product quality attribute. Qualification of equipment is pre-requisite for validation of the process in which the equipment is being used. Many types of equipment have measuring devices on them. Calibration of measuring devices is a part of qualification. Calibration of measuring devices is important, as the data is often collected through them. If the data collected is not from measuring devices that have been calibrated, the data cannot be relied upon. Thus the whole validation exercise can be questioned.
This was a presentation by me for a Seminar For My Pharm. Analysis class. I have tried well to include possible things but haven't gone much in deep because it would be irrelevant as per syllabus. If any mistakes, Please do leave a comment
HPLC is a High Performance liquid Chromatography.
High Pressure Liquid Chromatography.
High Priced Liquid Chromatography.
It is column chromatography.
It is Liquid Chromatography.
It is modified from of gas chromatography, it is applicable for both Volatile as well as Non volatile compound.
It can mainly divided by two types 1. Normal phase HPLC 2. Reversed Phase HPLC.
It is having a high resolution and separation capacity.
Dissolution as one of the most important aspects of Pharmaceutical dosage form showing the correlation between the in-vitro & in-vivo availability. Importance of dissolution, comparison with Disintegration, Sampling point, acceptance criteria as per Pharmacopoeias.
QUALIFICATION OF UV-VISIBLE SPECTROPHOTOMETER, FTIR, DSC, HPLCAnupriyaNR
Analytical method qualification consists of a simplified evaluation of a subset of validation characteristics with a goal to demonstrate that an analytical method is scientifically sound and suitable for its intended use. In contrast to validation, analytical method qualification is performed without predefined acceptability criteria. Qualification may be performed as a prerequisite to method validation, or when an assay for product knowledge has not yet been established as a test for a critical product quality attribute. Qualification of equipment is pre-requisite for validation of the process in which the equipment is being used. Many types of equipment have measuring devices on them. Calibration of measuring devices is a part of qualification. Calibration of measuring devices is important, as the data is often collected through them. If the data collected is not from measuring devices that have been calibrated, the data cannot be relied upon. Thus the whole validation exercise can be questioned.
This was a presentation by me for a Seminar For My Pharm. Analysis class. I have tried well to include possible things but haven't gone much in deep because it would be irrelevant as per syllabus. If any mistakes, Please do leave a comment
HPLC is a High Performance liquid Chromatography.
High Pressure Liquid Chromatography.
High Priced Liquid Chromatography.
It is column chromatography.
It is Liquid Chromatography.
It is modified from of gas chromatography, it is applicable for both Volatile as well as Non volatile compound.
It can mainly divided by two types 1. Normal phase HPLC 2. Reversed Phase HPLC.
It is having a high resolution and separation capacity.
Dissolution as one of the most important aspects of Pharmaceutical dosage form showing the correlation between the in-vitro & in-vivo availability. Importance of dissolution, comparison with Disintegration, Sampling point, acceptance criteria as per Pharmacopoeias.
Analytical method development and validation are one of the very imp aspects in Drug testing and approval process.Here I tried to explain the same with my experience.
HPLC Principle,Instrumentation and ApplicationAlakesh Pradhan
HPLC Chromatography and its principle
Liquid chromatography
High Performance Liquid Chromatography ( HPLC )
The components of the high performance liquid chromatograph (HPLC).
The separation process.
The chromatogram
Validation of uv visible spectrophotometer.pptxAnupamaCp2
Validation of UV-Visible spectrophotometer.
It includes installation qualification , design qualification, operational qualification, performance qualification.
University Institute of Pharmaceutical Sciences is a flag bearer of excellence in Pharmaceutical education and research in the country. Here is another initiative to make study material available to everyone worldwide. Based on the new PCI guidelines and syllabus here we have a presentation dealing with qualifications of HPLC which is the " High Performance Liquid Chromatography".
Thank you for reading.
Hope it was of help to you.
UIPS,PU team
qualification of instrument(UV & FTIR) BY Bhumi Suratiya, M.Pharm sem 2.pptxBhumiSuratiya
So, Here it's presentation on Qualification of instrument(UV & FTIR) BY Bhumi Suratiya, M.Pharm sem 2. Qualification of analytical instruments. it also includes design qualifications (DQ), Installation qualification(IQ)
Operational qualification(OQ)
Performance qualification(PQ).
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.
Prix Galien International 2024 Forum ProgramLevi Shapiro
June 20, 2024, Prix Galien International and Jerusalem Ethics Forum in ROME. Detailed agenda including panels:
- ADVANCES IN CARDIOLOGY: A NEW PARADIGM IS COMING
- WOMEN’S HEALTH: FERTILITY PRESERVATION
- WHAT’S NEW IN THE TREATMENT OF INFECTIOUS,
ONCOLOGICAL AND INFLAMMATORY SKIN DISEASES?
- ARTIFICIAL INTELLIGENCE AND ETHICS
- GENE THERAPY
- BEYOND BORDERS: GLOBAL INITIATIVES FOR DEMOCRATIZING LIFE SCIENCE TECHNOLOGIES AND PROMOTING ACCESS TO HEALTHCARE
- ETHICAL CHALLENGES IN LIFE SCIENCES
- Prix Galien International Awards Ceremony
Title: Sense of Taste
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 structure and function of taste buds.
Describe the relationship between the taste threshold and taste index of common substances.
Explain the chemical basis and signal transduction of taste perception for each type of primary taste sensation.
Recognize different abnormalities of taste perception and their causes.
Key Topics:
Significance of Taste Sensation:
Differentiation between pleasant and harmful food
Influence on behavior
Selection of food based on metabolic needs
Receptors of Taste:
Taste buds on the tongue
Influence of sense of smell, texture of food, and pain stimulation (e.g., by pepper)
Primary and Secondary Taste Sensations:
Primary taste sensations: Sweet, Sour, Salty, Bitter, Umami
Chemical basis and signal transduction mechanisms for each taste
Taste Threshold and Index:
Taste threshold values for Sweet (sucrose), Salty (NaCl), Sour (HCl), and Bitter (Quinine)
Taste index relationship: Inversely proportional to taste threshold
Taste Blindness:
Inability to taste certain substances, particularly thiourea compounds
Example: Phenylthiocarbamide
Structure and Function of Taste Buds:
Composition: Epithelial cells, Sustentacular/Supporting cells, Taste cells, Basal cells
Features: Taste pores, Taste hairs/microvilli, and Taste nerve fibers
Location of Taste Buds:
Found in papillae of the tongue (Fungiform, Circumvallate, Foliate)
Also present on the palate, tonsillar pillars, epiglottis, and proximal esophagus
Mechanism of Taste Stimulation:
Interaction of taste substances with receptors on microvilli
Signal transduction pathways for Umami, Sweet, Bitter, Sour, and Salty tastes
Taste Sensitivity and Adaptation:
Decrease in sensitivity with age
Rapid adaptation of taste sensation
Role of Saliva in Taste:
Dissolution of tastants to reach receptors
Washing away the stimulus
Taste Preferences and Aversions:
Mechanisms behind taste preference and aversion
Influence of receptors and neural pathways
Impact of Sensory Nerve Damage:
Degeneration of taste buds if the sensory nerve fiber is cut
Abnormalities of Taste Detection:
Conditions: Ageusia, Hypogeusia, Dysgeusia (parageusia)
Causes: Nerve damage, neurological disorders, infections, poor oral hygiene, adverse drug effects, deficiencies, aging, tobacco use, altered neurotransmitter levels
Neurotransmitters and Taste Threshold:
Effects of serotonin (5-HT) and norepinephrine (NE) on taste sensitivity
Supertasters:
25% of the population with heightened sensitivity to taste, especially bitterness
Increased number of fungiform papillae
The prostate is an exocrine gland of the male mammalian reproductive system
It is a walnut-sized gland that forms part of the male reproductive system and is located in front of the rectum and just below the urinary bladder
Function is to store and secrete a clear, slightly alkaline fluid that constitutes 10-30% of the volume of the seminal fluid that along with the spermatozoa, constitutes semen
A healthy human prostate measures (4cm-vertical, by 3cm-horizontal, 2cm ant-post ).
It surrounds the urethra just below the urinary bladder. It has anterior, median, posterior and two lateral lobes
It’s work is regulated by androgens which are responsible for male sex characteristics
Generalised disease of the prostate due to hormonal derangement which leads to non malignant enlargement of the gland (increase in the number of epithelial cells and stromal tissue)to cause compression of the urethra leading to symptoms (LUTS
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!
Couples presenting to the infertility clinic- Do they really have infertility...Sujoy Dasgupta
Dr Sujoy Dasgupta presented the study on "Couples presenting to the infertility clinic- Do they really have infertility? – The unexplored stories of non-consummation" in the 13th Congress of the Asia Pacific Initiative on Reproduction (ASPIRE 2024) at Manila on 24 May, 2024.
- 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
Factory Supply Best Quality Pmk Oil CAS 28578–16–7 PMK Powder in Stockrebeccabio
Factory Supply Best Quality Pmk Oil CAS 28578–16–7 PMK Powder in Stock
Telegram: bmksupplier
signal: +85264872720
threema: TUD4A6YC
You can contact me on Telegram or Threema
Communicate promptly and reply
Free of customs clearance, Double Clearance 100% pass delivery to USA, Canada, Spain, Germany, Netherland, Poland, Italy, Sweden, UK, Czech Republic, Australia, Mexico, Russia, Ukraine, Kazakhstan.Door to door service
Hot Selling Organic intermediates
Tom Selleck Health: A Comprehensive Look at the Iconic Actor’s Wellness Journeygreendigital
Tom Selleck, an enduring figure in Hollywood. has captivated audiences for decades with his rugged charm, iconic moustache. and memorable roles in television and film. From his breakout role as Thomas Magnum in Magnum P.I. to his current portrayal of Frank Reagan in Blue Bloods. Selleck's career has spanned over 50 years. But beyond his professional achievements. fans have often been curious about Tom Selleck Health. especially as he has aged in the public eye.
Follow us on: Pinterest
Introduction
Many have been interested in Tom Selleck health. not only because of his enduring presence on screen but also because of the challenges. and lifestyle choices he has faced and made over the years. This article delves into the various aspects of Tom Selleck health. exploring his fitness regimen, diet, mental health. and the challenges he has encountered as he ages. We'll look at how he maintains his well-being. the health issues he has faced, and his approach to ageing .
Early Life and Career
Childhood and Athletic Beginnings
Tom Selleck was born on January 29, 1945, in Detroit, Michigan, and grew up in Sherman Oaks, California. From an early age, he was involved in sports, particularly basketball. which played a significant role in his physical development. His athletic pursuits continued into college. where he attended the University of Southern California (USC) on a basketball scholarship. This early involvement in sports laid a strong foundation for his physical health and disciplined lifestyle.
Transition to Acting
Selleck's transition from an athlete to an actor came with its physical demands. His first significant role in "Magnum P.I." required him to perform various stunts and maintain a fit appearance. This role, which he played from 1980 to 1988. necessitated a rigorous fitness routine to meet the show's demands. setting the stage for his long-term commitment to health and wellness.
Fitness Regimen
Workout Routine
Tom Selleck health and fitness regimen has evolved. adapting to his changing roles and age. During his "Magnum, P.I." days. Selleck's workouts were intense and focused on building and maintaining muscle mass. His routine included weightlifting, cardiovascular exercises. and specific training for the stunts he performed on the show.
Selleck adjusted his fitness routine as he aged to suit his body's needs. Today, his workouts focus on maintaining flexibility, strength, and cardiovascular health. He incorporates low-impact exercises such as swimming, walking, and light weightlifting. This balanced approach helps him stay fit without putting undue strain on his joints and muscles.
Importance of Flexibility and Mobility
In recent years, Selleck has emphasized the importance of flexibility and mobility in his fitness regimen. Understanding the natural decline in muscle mass and joint flexibility with age. he includes stretching and yoga in his routine. These practices help prevent injuries, improve posture, and maintain mobilit
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
HOT NEW PRODUCT! BIG SALES FAST SHIPPING NOW FROM CHINA!! EU KU DB BK substit...GL Anaacs
Contact us if you are interested:
Email / Skype : kefaya1771@gmail.com
Threema: PXHY5PDH
New BATCH Ku !!! MUCH IN DEMAND FAST SALE EVERY BATCH HAPPY GOOD EFFECT BIG BATCH !
Contact me on Threema or skype to start big business!!
Hot-sale products:
NEW HOT EUTYLONE WHITE CRYSTAL!!
5cl-adba precursor (semi finished )
5cl-adba raw materials
ADBB precursor (semi finished )
ADBB raw materials
APVP powder
5fadb/4f-adb
Jwh018 / Jwh210
Eutylone crystal
Protonitazene (hydrochloride) CAS: 119276-01-6
Flubrotizolam CAS: 57801-95-3
Metonitazene CAS: 14680-51-4
Payment terms: Western Union,MoneyGram,Bitcoin or USDT.
Deliver Time: Usually 7-15days
Shipping method: FedEx, TNT, DHL,UPS etc.Our deliveries are 100% safe, fast, reliable and discreet.
Samples will be sent for your evaluation!If you are interested in, please contact me, let's talk details.
We specializes in exporting high quality Research chemical, medical intermediate, Pharmaceutical chemicals and so on. Products are exported to USA, Canada, France, Korea, Japan,Russia, Southeast Asia and other countries.
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.
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.
3. Introduction
Analytical instruments are used for a specific analysis of
drugs and pharmaceuticals.
So, regular performance verification are made to ensure
that the instruments used in the analytical purpose should be
properly validated and calibrated “to demonstrate that it is
suitable for its intended purpose”.
4. Calibration
Calibration is a process by which ensure that an
instrument readings are accurate with reference to established
standards.
Calibration is performed using primary reference
standards.
Instruments need to be calibrated before using.
For example- weighing balance,p
H
meter,…….etc
5. Need for calibration
Calibration can be called for:
with a new instrument.
when a specified time period is elapsed.
when a specified usage (operating hours) has elapsed.
when an instrument has had a shock or vibration which
potentially may have put it out of calibration.
sudden changes in weather.
whenever observations appear questionable.
6. Validation
Validation is a detailed process of confirming that the
instrument is installed correctly, that it is operating effectively,
and that it is performing without error.
The field of validation is divided into a number of
subsections as follows-
Cleaning validation
Process validation
Analytical method validation
Computer system validation
7. Equipment validation
It demonstrate that equipment used in validation studies is
suitable for use and is comparable to equipment used for routine
analysis.
Qualification
Action of proving and documenting that equipment or
ancillary systems are properly installed, work correctly, and actually
lead to the expected results.
Qualification is part of validation , but the individual
qualification steps alone do not constitute process validation.
8. Parts of qualification
The activity of qualifying system of equipment is
divided into four subtypes-
Design qualification (DQ)
Installation qualification (IQ)
Operational qualification (OQ)
Performance qualification (PQ)
9. Design qualification (DQ)- Demonstrates that the
proposed design will satisfy all the requirements that
are defined and detailed in the User Requirements
Specification.
Installation qualification (IQ)- Demonstrates that the
process or equipment meets all specifications, is
installed correctly, and all required components and
documentation needed for continued operation are
installed and in place.
10. Operational qualification (OQ)- Demonstrates that all
facets of the process or equipment are operating correctly.
Performance qualification (PQ)- Demonstrates that the
process or equipment performs as intended in a consistent
manner over time.
14. Wavelength accuracy:-
It is defined as the deviation of the wavelength reading at an
absorption band or emission band from the wavelength of the band.
15. Test:-
Wavelength accuracy verification is checked by comparing the recorded
wavelength of the peak against the value of reference standard.
commonly used wavelength standards such as
Deuterium lamp,
Mercury vapor lamp,
Holmium oxide filter, and
Holmium oxide solution (4% holmium oxide in 10% perchloric acid in a 1-cm
cell)
16. Acceptance
±1 nm in the UV range (200 to 380 nm) and
±3 nm in the visible range (380 to 800 nm).
Three repeated scans of the same peak should be within ±0.5 nm.
•
17. Stray light:-
Stray light is defined as the detected light of any wavelength that is
outside the bandwidth of the wavelength selected.
Test:-
Three test solutions prepared and measured the stray light at 200 nm,
220 nm and 340 nm
Acceptance:-
The transmittance of the solution in a 1 cm cell should be less than 0.01
or the absorbance value should be greater than 2.
18. At 1% transmittance, stray light at 1% of the
incident light intensity can cause a 15% drop in absorbance
19. Resolution power:-
The resolution of a UV-VIS spectrophotometer is related to its
spectral bandwidth(SBW).The smaller the spectral width, the finer the
resolution.
The SBW depends on the slit width and the dispersive power of the
monochromator
Test:-
0.02%v/v toluene in hexane is used to test the resolution power of the
spectrophotometer. The absorbance measured at 269 nm and 266 nm.
Acceptance:-
The ratio of the absorbance at 269 nm and absorbance at 266 nm
should be grater than 1.5
20.
21. Noise:-
Noise in the measurement affects the accuracy at both ends of
the absorbance scale.
Photon noise from the light source affects the accuracy of the
measurements leads to low absorbance.
Test:-
Air is scanned in the absorbance mode for 10 min.peak to noise
is recorded at 500nm.Root mean square noise is then calculated.
Acceptance:-
The RMS noise should be less than 0.001 AU
22.
23. Baseline flatness:-
The flat baseline test demonstrates the ability of the instrument to
normalize the light intensity measurement and the spectral output at
different wavelengths through out the spectral range.
Test:-
Air is scanned in the absorbance mode.The highest and lowest
deflections in the absorbance unit are recorded.
Acceptance:-
The deflection is typically less than 0.01AU
24.
25. Stability:-
The lamp intensity is a function of the age of the lamp,
temperature fluctuation, and wavelength of the measurement.
These changes can lead to errors in the value of the measurements,
over an extended period of time.
Test:-
Air is scanned in the absorbance mode for 60 min at specific
wavelength(340nm).The highest and lowest deflections in the absorbance
unit are recorded.
Acceptance:-
The deflection is less than 0.002 AU/h
26.
27. Photometric accuracy:-
Photometric accuracy is determined by comparing the difference
between the measured absorbance of the reference materials and the
established value.
Test:-
Either neutral density filters or potassium dichromate solutions
are used.
Acceptance:-
Six replicate measurements of the 0.006%w/v potassium
dichromate solution at 235, 257, 313 and 350 nm should be less than 0.5%
RSD.
28.
29. Linearity:-
The linear dynamic range of the measurement is limited by stray
light at high absorbance and by noise at low absorbance.
The accuracy of the quanitification of the sample depends on the
precision and linearity of the measurements.
Test:-
A series of Potassium dichromate solution of concentration
20,40,60,80 and 100mg/L in 0.005M sulfuric acid. The absorption of
various wavelength are plotted against the concentration of the solution
and the correlation coefficients are calculated.
Acceptance:-
Correlation coefficient r≥ 0.999
30. Calibration of IR spectrophotometer
Wave number verification
Resolution performance
31. Wave number verification:-
Prepare polystyrene film with thickness 0.04 mm and verify
the wavenumber
Observed
wavenumber
Minimum
tolerance
Maximum
tolerance
3058.5 3061.5
2848.0 2851.0
1941.4 1944.4
1600.2 1602.2
1582.0 1584.0
1153.5 1155.5
1027.3 1029.3
33. Calibration of spectrofluorimeter
Sensitivity of the instrument checked by using
primary standard
Prepare 1ppm solution of quinine sulphate
solution in 0.1M sulphuric acid.
Primary wavelength set at 366 nm, and check
the sensitivity of the instrument.
36. Flow rate accuracy:-
The perfoemance of pump module is the ability to maintain
accurate and consistent flow of the mobile phase.Poor flow rate will affect
the retention time and resolution of the separation.
Test:-
The flow rate accuracy at 2 ml/min can be verified by using a calibrated
stopwatch to measure the time it takes to collect 25 ml of effluent from the
pump into a 25 ml volumetric flask
Acceptance:-
±2.0% 0f the set flow rate
37. Gradient accuracy
The accuracy and linearity of the gradient solvent delivery can be
verified indirectly by monitoring the absorbance change when the
composition of the two solvents from two different channels changes.
TEST
Channel A is filled with a pure solvent such as methanol and
Channel B is filled with a solvent containing a UV-active tracer such as
caffeine (ca. 15 mg per liter of solvent).
38. The gradient profile is programmed to vary the composition of the
mixture from 100% A to 100% B in a short period of time, and then
changed back to 100% A in a stepwise manner.
If the composition of the 20% A and 80% B mixture is accurate, the
height B1 , which corresponds to the absorbance at 80% B
The linearity of the gradient delivery can be verified
by plotting the absorbance at various mobile-phase composition versus
sample compositions.
39. System precision:-
Weigh accurately 60 mg of caffeine into 100 ml volumetric flask.
Dissolve and dilute to the volume with mobile phase.Transfer 10
ml of this solution into 100 ml flask and make up with mobile phase.
Inject blank followed by standard preparation in 6 replicates.
Note down the areas and retention times.
Acceptance:-
The % RSD of retention time and peak area should be <1.0%
40. Wavelength accuracy:-
Inject blank followed by standard preparation and note down
the height or absorbance.
Acceptance:-
The maximum absorbance should be ±2 nm.
41. Detector linearity:-
The linearity of the detector response can be checked by pumping or by
filling the flow cell with a series of standard solution of various
concentration.
Aqueous caffeine solutions are convenient for the linearity
measurement.
The correlation coefficient between sample concentration and response
can be calculated to determine the linearity.
Acceptance:-
R≥ 0.999
42. Injector linearity:-
Linearity is important for methods that require the use of variable
injection volumes.
The linearity of the injector can be demonstrated by making injections,
typically 5,10,20,50 and 100 μl to cover the range 0 to 100 μl.
The response of the injection is plotted against the injection volume.
The correlation coefficient of the plot is used in evaluation of the injector
linearity.
Acceptance:-
R≥0.999
43. Column oven temperature accuracy:-
The efficiency of HPLC column varies with column temperature.
The temperature accuracy of the column heater is evaluated by placing a
calibrated thermometer in the column compartment to measure
the actual compartment temperature.
The thermometer readings are compared to the preset temperature at 40
and 60°C.
Acceptance:-
The resulting oven temperature from the thermometer display
should be within ±2°C of the set temperature.
45. Spotting & Detection capacity:-
Requirements:-
Alumina glass plates
Sodium salicylate
96%v/v alcohol
Preparation of stock solution:-
Stock solution-1
Weigh 500 mg of sodium salicylate in 250 ml volumetric flask
dissolve and dilute with 96%v/v alcohol.
Stock solution-2
100 mg of sod.salicylate in 250 ml volumetric flask, dissolve and
dilute with 96% v/v alcohol.
46. Procedure:-
Spot 5μl of each solution observe at 254 nm, 366 nm.
Acceptance:-
The spots shall be comparable intensity wise.
Spot due to stock solution-2 shall be visible at 254 nm.
Spot due to stock solution-1 shall be visible at 366 nm.
47. Calibration of Gas chromatography
Flow rate accuracy
Column oven temperature accuracy
System precision
System precision for head space auto sampler
Detector linearity
Detector noise and drift test
48. Flow rate accuracy:-
Connect the digital flow meter to the detector outlet port.
Set the carrier gas flow and wait till it reaches the set flow.
Note the observed flow in replicate.
Repeat the procedure for other carrier gases such as Hydrogen
and Air.
Acceptance
The flow rate of carrier gas should be ±10% of set flow.
S.No Carrier gas Acceptance
criteria in
ml/mt
1. Helium 125
2. Hydrogen 40
3. Air 400
49. Column oven temperature accuracy
Place the thermometer in the column oven and set the column
oven temperature at 40°C.Wait till the temperature stabilizes.
Note the observed temperature over a period of 10 mts.
Repeat the procedure for 100°C, 150°C and 190°C.
Acceptance
The resulting oven temperature from the thermometer display
should be within ±2°C of the set temperature.
50. System precision
Transfer 20 ml of methanol,Ethanol and acetone into 100 ml
volumetric flask and make up with ethyl acetate.
Inject blank followed by standard preparation in 6
replicates.Note down the areas and retention times.
Acceptance
The %RSD of retention time should be not more than 1.0% &
peak area NMT 5.0%
51. System precision for head space auto sampler
Prepare a standard mixture solution Methylene
dichloride(0.6g),Chloroform(0.06g),Trichloroethane(0.08g),1,4,Dioxane
0.38g) in 50 ml volumetric flask containing 40 ml of Dimethyl
formamide.
Finally make upto the volume with DMF(Solution-A).
52. Take 0.5 ml of standard solution A in 6 different vials and seal caps and crimp.
Place these vials on head space sampler. Prepare a blank vial also.
Load the vials in head space sampler tray.
Blank vials followed by the standard vials.
Acceptance
The %RSD of retention time should be NMT 1.0% and Peak area should b
NMT 15.0%
53. Detector linearity
Detector linearity solutions
10 ml of
Methanol
,Ethanol,
Acetone
make up
to 100 ml
with
Ethyl
acetate
15ml of
Methanol
,Ethanol,
Acetone
make up
to 100 ml
with
Ethyl
acetate
20ml of
Methanol
,Ethanol,
Acetone
make up
to 100 ml
with
Ethyl
acetate
25ml of
Methanol
,Ethanol,
Acetone
make up
to 100 ml
with
Ethyl
acetate
30 ml of
Methanol,
Ethanol,
Acetone
make up
to 100 ml
with
Ethyl
acetate
Solution A Solution B Solution C Solution D Solution E
54. Procedure:-
Inject blank,followed by detector linearity solutions
and record the peak responses.
Draw a standard plot between the concentration Vs
the peak responses.
Acceptance
The plot should be linear and regression coefficient
should NLT 0.99
55. Detector noise and Drift test:-
After GC is ready run the system upto 15mts through
single run. After completion of run calculate noise and drift
through software.
Acceptance
Noise NMT 100 μV
Drift NMT 2500μV/hr
56. Schedule for calibration of major instruments
INSTRUMENT INTERVAL(MONTHS)
HPLC 3 ± 7 days
Gas chromatography 3 ± 7 days
UV-Visible spectrophotometer Monthly once ± 3 days
IR spectrophotometer Monthly once ± 3 days
NMR spectrophotometer 6 ± 15 days
Flourimeter 3 ± 7 days
pH meter Daily
Analytical Balance Daily
57. References:-
Journal of Biomedical sciences and research-volume 2(2),
2010, page no:- 89-99.
Practical pharmaceutical chemistry by A.H.Beckett,
J.B.Stenlake, Part Two, page no:- 326.
Analytical Method Validation And Instrument Performance
Verification by Herman lam., page no:- 153-186.