ICP-MS and ICP-AES are the preferred techniques for determining elemental impurities in pharmaceuticals according to recent ICH guidelines. ICP-MS can detect impurities below the ppt level, outperforming other techniques like GF-AAS (ppb range) and ICP-AES (ppb range). Speciation is important as different forms can have different toxicities, and ICP-MS coupled with separation techniques can perform speciation analysis down to ppt levels for quality control of pharmaceutical products.
MASS SPECTROMETRY(mass-spec) -2013 - P.ravisankar- WHAT ABOUT MASS SPECTROMET...Dr. Ravi Sankar
MASS SPECTROMETRY(mass-spec) -2013 - P.ravisankar-WHAT ABOUT MASS SPECTROMETRY,BASIC PRINCIPLE,INSTRUMENTATION, ION SOURCES, MASS ANALYZERS,APPLICATIONS.
P.RAVISANKAR, VIGNAN PHARMACY COLLEGE, VADLAMUDI
MASS SPECTROMETRY(mass-spec) -2013 - P.ravisankar- WHAT ABOUT MASS SPECTROMET...Dr. Ravi Sankar
MASS SPECTROMETRY(mass-spec) -2013 - P.ravisankar-WHAT ABOUT MASS SPECTROMETRY,BASIC PRINCIPLE,INSTRUMENTATION, ION SOURCES, MASS ANALYZERS,APPLICATIONS.
P.RAVISANKAR, VIGNAN PHARMACY COLLEGE, VADLAMUDI
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.
Mass spectrometer converts molecules to ions under vacuum so that they can be moved about and manipulated by external electric and magnetic fields.
These ions are then separated and determined. Separation is achieved on different trajectories of moving ions in electrical and/or magnetic fields.
*Electrospray Ionization (ESI)
*Matrix-Assisted Laser Desorption/Ionization (MALDI)
*Time-of-Flight (TOF) Mass Analyzer
Recent advances in the application of mass spectrometry in food-related analysis
*LC-MS coupling techniques
*HPLC-MS coupling techniques
*MALDI-TOF-MS
*ESI-MS
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis), 1st semester.
*not all topics have been covered in this file.
Different forms of an element can exhibit very different physicochemical properties, including varying toxicities. The chromatography process of separation and quantification of different chemical forms of an element, more specifically termed speciation analysis, can be utilized to determine an element’s various chemical forms. The food safety industries have significantly increased their interest in understanding an element’s various chemical forms due to pending legislative pressures. Learn about the latest developments in speciation technology and offer proof data for a wide variety of applications, including arsenic species in apple juice and rice syrup and iodine species in milk.
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.
Mass spectrometer converts molecules to ions under vacuum so that they can be moved about and manipulated by external electric and magnetic fields.
These ions are then separated and determined. Separation is achieved on different trajectories of moving ions in electrical and/or magnetic fields.
*Electrospray Ionization (ESI)
*Matrix-Assisted Laser Desorption/Ionization (MALDI)
*Time-of-Flight (TOF) Mass Analyzer
Recent advances in the application of mass spectrometry in food-related analysis
*LC-MS coupling techniques
*HPLC-MS coupling techniques
*MALDI-TOF-MS
*ESI-MS
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis), 1st semester.
*not all topics have been covered in this file.
Different forms of an element can exhibit very different physicochemical properties, including varying toxicities. The chromatography process of separation and quantification of different chemical forms of an element, more specifically termed speciation analysis, can be utilized to determine an element’s various chemical forms. The food safety industries have significantly increased their interest in understanding an element’s various chemical forms due to pending legislative pressures. Learn about the latest developments in speciation technology and offer proof data for a wide variety of applications, including arsenic species in apple juice and rice syrup and iodine species in milk.
In the past, measuring the total amount of an element was sufficient. Unfortunately, the effects of an element extend far beyond its absolute amount. Different forms of an element can exhibit very different physicochemical properties, including varying toxicities. The process of separation and quantification of different chemical forms of an element, more specifically termed speciation analysis, can be utilized to determine an element’s various chemical forms. The number of environmental applications of elemental speciation analysis has increased significantly. For example, both the United States EPA and the European Union have specified maximum admissible chromium concentrations in their respective drinking water directives and are evaluating the inclusion of hexavalent chromium in certain legislation. Learn about the latest developments in chromatography technology for speciation analysis that offer data for a wide variety of applications, including chromium in drinking water and both arsenic and sulfur in environmental waters.
Gas chromatography-mass spectrometry (GC-MS) is the synergistic combination of two analytical method to separate and identify different substances within a test sample.
Gas chromatography separates the components of a mixture in time.
Mass spectrometer provides information that aids in the identification and structural elucidation of each component.
AAS is an analytical technique used to determine how much of certain elements are in a sample. It uses the principle that atoms (and ions) can absorb light at a specific, unique wavelength. When this specific wavelength of light is provided, the energy (light) is absorbed by the atom.
THE IMPORTANCE OF MARTIAN ATMOSPHERE SAMPLE RETURN.Sérgio Sacani
The return of a sample of near-surface atmosphere from Mars would facilitate answers to several first-order science questions surrounding the formation and evolution of the planet. One of the important aspects of terrestrial planet formation in general is the role that primary atmospheres played in influencing the chemistry and structure of the planets and their antecedents. Studies of the martian atmosphere can be used to investigate the role of a primary atmosphere in its history. Atmosphere samples would also inform our understanding of the near-surface chemistry of the planet, and ultimately the prospects for life. High-precision isotopic analyses of constituent gases are needed to address these questions, requiring that the analyses are made on returned samples rather than in situ.
This pdf is about the Schizophrenia.
For more details visit on YouTube; @SELF-EXPLANATORY;
https://www.youtube.com/channel/UCAiarMZDNhe1A3Rnpr_WkzA/videos
Thanks...!
(May 29th, 2024) Advancements in Intravital Microscopy- Insights for Preclini...Scintica Instrumentation
Intravital microscopy (IVM) is a powerful tool utilized to study cellular behavior over time and space in vivo. Much of our understanding of cell biology has been accomplished using various in vitro and ex vivo methods; however, these studies do not necessarily reflect the natural dynamics of biological processes. Unlike traditional cell culture or fixed tissue imaging, IVM allows for the ultra-fast high-resolution imaging of cellular processes over time and space and were studied in its natural environment. Real-time visualization of biological processes in the context of an intact organism helps maintain physiological relevance and provide insights into the progression of disease, response to treatments or developmental processes.
In this webinar we give an overview of advanced applications of the IVM system in preclinical research. IVIM technology is a provider of all-in-one intravital microscopy systems and solutions optimized for in vivo imaging of live animal models at sub-micron resolution. The system’s unique features and user-friendly software enables researchers to probe fast dynamic biological processes such as immune cell tracking, cell-cell interaction as well as vascularization and tumor metastasis with exceptional detail. This webinar will also give an overview of IVM being utilized in drug development, offering a view into the intricate interaction between drugs/nanoparticles and tissues in vivo and allows for the evaluation of therapeutic intervention in a variety of tissues and organs. This interdisciplinary collaboration continues to drive the advancements of novel therapeutic strategies.
A brief information about the SCOP protein database used in bioinformatics.
The Structural Classification of Proteins (SCOP) database is a comprehensive and authoritative resource for the structural and evolutionary relationships of proteins. It provides a detailed and curated classification of protein structures, grouping them into families, superfamilies, and folds based on their structural and sequence similarities.
Richard's aventures in two entangled wonderlandsRichard Gill
Since the loophole-free Bell experiments of 2020 and the Nobel prizes in physics of 2022, critics of Bell's work have retreated to the fortress of super-determinism. Now, super-determinism is a derogatory word - it just means "determinism". Palmer, Hance and Hossenfelder argue that quantum mechanics and determinism are not incompatible, using a sophisticated mathematical construction based on a subtle thinning of allowed states and measurements in quantum mechanics, such that what is left appears to make Bell's argument fail, without altering the empirical predictions of quantum mechanics. I think however that it is a smoke screen, and the slogan "lost in math" comes to my mind. I will discuss some other recent disproofs of Bell's theorem using the language of causality based on causal graphs. Causal thinking is also central to law and justice. I will mention surprising connections to my work on serial killer nurse cases, in particular the Dutch case of Lucia de Berk and the current UK case of Lucy Letby.
Professional air quality monitoring systems provide immediate, on-site data for analysis, compliance, and decision-making.
Monitor common gases, weather parameters, particulates.
What is greenhouse gasses and how many gasses are there to affect the Earth.moosaasad1975
What are greenhouse gasses how they affect the earth and its environment what is the future of the environment and earth how the weather and the climate effects.
Richard's entangled aventures in wonderlandRichard Gill
Since the loophole-free Bell experiments of 2020 and the Nobel prizes in physics of 2022, critics of Bell's work have retreated to the fortress of super-determinism. Now, super-determinism is a derogatory word - it just means "determinism". Palmer, Hance and Hossenfelder argue that quantum mechanics and determinism are not incompatible, using a sophisticated mathematical construction based on a subtle thinning of allowed states and measurements in quantum mechanics, such that what is left appears to make Bell's argument fail, without altering the empirical predictions of quantum mechanics. I think however that it is a smoke screen, and the slogan "lost in math" comes to my mind. I will discuss some other recent disproofs of Bell's theorem using the language of causality based on causal graphs. Causal thinking is also central to law and justice. I will mention surprising connections to my work on serial killer nurse cases, in particular the Dutch case of Lucia de Berk and the current UK case of Lucy Letby.
Slide 1: Title Slide
Extrachromosomal Inheritance
Slide 2: Introduction to Extrachromosomal Inheritance
Definition: Extrachromosomal inheritance refers to the transmission of genetic material that is not found within the nucleus.
Key Components: Involves genes located in mitochondria, chloroplasts, and plasmids.
Slide 3: Mitochondrial Inheritance
Mitochondria: Organelles responsible for energy production.
Mitochondrial DNA (mtDNA): Circular DNA molecule found in mitochondria.
Inheritance Pattern: Maternally inherited, meaning it is passed from mothers to all their offspring.
Diseases: Examples include Leber’s hereditary optic neuropathy (LHON) and mitochondrial myopathy.
Slide 4: Chloroplast Inheritance
Chloroplasts: Organelles responsible for photosynthesis in plants.
Chloroplast DNA (cpDNA): Circular DNA molecule found in chloroplasts.
Inheritance Pattern: Often maternally inherited in most plants, but can vary in some species.
Examples: Variegation in plants, where leaf color patterns are determined by chloroplast DNA.
Slide 5: Plasmid Inheritance
Plasmids: Small, circular DNA molecules found in bacteria and some eukaryotes.
Features: Can carry antibiotic resistance genes and can be transferred between cells through processes like conjugation.
Significance: Important in biotechnology for gene cloning and genetic engineering.
Slide 6: Mechanisms of Extrachromosomal Inheritance
Non-Mendelian Patterns: Do not follow Mendel’s laws of inheritance.
Cytoplasmic Segregation: During cell division, organelles like mitochondria and chloroplasts are randomly distributed to daughter cells.
Heteroplasmy: Presence of more than one type of organellar genome within a cell, leading to variation in expression.
Slide 7: Examples of Extrachromosomal Inheritance
Four O’clock Plant (Mirabilis jalapa): Shows variegated leaves due to different cpDNA in leaf cells.
Petite Mutants in Yeast: Result from mutations in mitochondrial DNA affecting respiration.
Slide 8: Importance of Extrachromosomal Inheritance
Evolution: Provides insight into the evolution of eukaryotic cells.
Medicine: Understanding mitochondrial inheritance helps in diagnosing and treating mitochondrial diseases.
Agriculture: Chloroplast inheritance can be used in plant breeding and genetic modification.
Slide 9: Recent Research and Advances
Gene Editing: Techniques like CRISPR-Cas9 are being used to edit mitochondrial and chloroplast DNA.
Therapies: Development of mitochondrial replacement therapy (MRT) for preventing mitochondrial diseases.
Slide 10: Conclusion
Summary: Extrachromosomal inheritance involves the transmission of genetic material outside the nucleus and plays a crucial role in genetics, medicine, and biotechnology.
Future Directions: Continued research and technological advancements hold promise for new treatments and applications.
Slide 11: Questions and Discussion
Invite Audience: Open the floor for any questions or further discussion on the topic.
This presentation explores a brief idea about the structural and functional attributes of nucleotides, the structure and function of genetic materials along with the impact of UV rays and pH upon them.
Observation of Io’s Resurfacing via Plume Deposition Using Ground-based Adapt...Sérgio Sacani
Since volcanic activity was first discovered on Io from Voyager images in 1979, changes
on Io’s surface have been monitored from both spacecraft and ground-based telescopes.
Here, we present the highest spatial resolution images of Io ever obtained from a groundbased telescope. These images, acquired by the SHARK-VIS instrument on the Large
Binocular Telescope, show evidence of a major resurfacing event on Io’s trailing hemisphere. When compared to the most recent spacecraft images, the SHARK-VIS images
show that a plume deposit from a powerful eruption at Pillan Patera has covered part
of the long-lived Pele plume deposit. Although this type of resurfacing event may be common on Io, few have been detected due to the rarity of spacecraft visits and the previously low spatial resolution available from Earth-based telescopes. The SHARK-VIS instrument ushers in a new era of high resolution imaging of Io’s surface using adaptive
optics at visible wavelengths.
3. Introduction
• Toxic metals like As, Pb, Cd, Hg, Se, Cr, Al, Ni, Cu and U enter
the human body via the food chain including medicines, ambient
air and drinking water leading to health problems.
• In addition, metal ions also can affect the stability and shelf life
of the formulation, catalyze the degradation of the API’s
leading to the formation of unqualified degradates
• Recently ICH has proposed safety standard guidelines for metal
impurities (Q3D) for the purpose of quality assurance of
pharmaceutical products
4.
5.
6.
7. What is Speciation analysis ?
• Speciation analysis was first described in 1993 by Forstner
• The process of separation and quantification of different
chemical forms of an element is more specifically termed
speciation analysis.
• Inorganic As is much more toxic than the common organic
forms, such as arsenobetaine, (the sum of arsenite (As(III))
and arsenate (As(V)) is below the limit.
• Similarly, the Hg limit is based on inorganic Hg (Hg2+),
although methyl mercury (MeHg) is the more toxic form. The
presence of MeHg in pharmaceuticals is considered unlikely, but
it should be separated and measured specifically if samples are
derived from material (for example, fish tissue) that may
contain the compound in significant amounts.
8.
9. • Distribution, Mobility, Bioavailability and Toxicity of
trace metals in environmental and biological systems
depend not simply on their concentrations, but
critically on their chemical forms
• Individual metal species posses different chemical
activity and ability to transform
• Speciation techniques using ICP-MS, ICP-AES, could
be considered as the most sensitive and selective
techniques
12. Atomic absorption
spectrometry (AAS)
• This technique is based on the principle that the amount of light
absorbed is a measure of the concentration of a particular analyte
at a particular wavelength
• GF-AAS is a technique which involves injection of a small amount
of solution to be analyzed into a small graphite tube and thus is
suitable for the analysis of metals at ultra-trace levels
• Mercury by ‘cold vapor’ method and some ‘volatile’ elements like
As and Sb can be measured as their hydrides . A major advantage
of cold vapor-AAS is the inherent separation of mercury from
the matrix .
13.
14. Both F-AAS and GF-AAS allow reliable determination of metallic impurities
in pharmaceutical quality control operations.
15. Instrumental neutron activation analysis
(INAA)
• INAA is a relatively straightforward analytical technique for
determining elemental abundance in a wide range of materials.
• This technique relies on the measurement of characteristic radiation
from radionuclides formed directly or indirectly by neutron irradiation
of the material of interest. The energy of the emitted gamma rays is
used to identify the nuclide and the intensity of the radiation can be
used to determine its abundance.
16. • The advantages include,
I. The method is non-destructive, hence the same sample can be
used for other measurements;
II. Sample size can be very small, often as little as a milligram;
III. Detection limits for many elements are in the ng/g range;
IV. No sample preparation is required; and
V. Over 40 elements can be measured simultaneously.
• Because of these advantages, INAA used to be a very popular
analytical technique compared to other analytical methods until
ICPMS came in to use.
• As NAA does not require sample dissolution, it has a great advantage
over solution techniques such as AAS, ICPAES and ICP-MS.
• Despite the above advantages, INAA is certainly not a popular
analytical technique as it is time-consuming, not independent, requires a
reactor nearby and involves longer cooling times for certain elements.
17. X-ray florescence spectrometry
(XRF)
• In recent times XRF analysis
has become increasingly
attractive when compared to
other techniques, especially
due to the ease of sample
preparation.
• XRF spectrometry involves
irradiation of the sample
with high energy excitation
X-rays and measurement of
element-specific
fluorescence X-rays at a
particular wavelength or
energy from the sample .
Samples can be in solid,
powder or liquid form.
18. • Since it is a non-contact analysis, problems such as memory effects
commonly experienced in solution analysis, are not encountered.
• As it is a non-destructive technique, it is possible to reuse the
sample after measurements.
• Both forms, namely, wavelength dispersive-XRF (WD-XRF) and
energy dispersive-XRF (EDXRF) techniques have been successfully
applied for the determination of Zn, Fe and Ni in API’s .
• Though there are several studies on the application of XRF
techniques in pharmaceutical industry, because of the higher
detection limits, they are not very popular for quantitative
determinations of metal impurities in pharmaceutical samples.
19. Inductively Coupled Plasma
What is a Plasma?
•Plasma source provides atomization
•Plasma: “a gas-like phase of matter that
consists of charged particles”
•ICP-AES plasma source is from the carrier
gas
Typically argon is used
20. • ICP is a very powerful ionisation source
• Elements with IP < 8 eV are ionised to > 90%
• LODs for most metals are <ppb level
• Sample introduction is very versatile: liquid, gaseous or even
solid samples can be ionised in the Plasma
• The sample introduction allows a (relatively) straightforward
coupling of chromatographic separation systems (GC, HPLC)
• ICP-MS detection is fast and multi-element capable
• A large variety of element speciation tasks can be tackled by
GC or HPLC coupled to ICP-MS
21. • ICP-AES technique involves measurement of light emitted by
the elements in a sample when introduced into an ICP source.
• The measured emission intensities are then compared to the
intensities of standards of known concentrations to obtain the
respective elemental concentrations in an unknown sample .
.
Inductively Coupled Plasma Atomic
Emission Spectrometry (ICP-AES)
22. • Limits of detection were at least a factor of ten below the USP
limit concentrations confirming that the ICP-AES technique is
well suited for quantitative determination of elemental impurities
in pharmaceutical samples.
•The technique can simultaneously measure up to 60 elements
with high sensitivity and an extraordinarily wide linear dynamic
range which is perhaps the most outstanding feature of the ICP-
AES
• The general chapter USP <233> includes two analytical
procedures involving ICP-AES and ICP-MS for determination of
elemental impurities in pharmaceuticals and includes a
comprehensive validation procedure to ensure acceptability of
results .
• Compared with F-AAS, ICP-AES provides lower detection limits,
has multielement capability and a wider linear dynamic range
23. Inductively coupled plasma mass
spectrometry (ICP-MS)
ICP-MS combines a high-temperature ICP source with a mass
spectrometer. The ICP source converts atoms of the elements in the
sample to positively charged ions. These ions separated on the basis
of mass-to-charge ratio in a mass spectrometer, are directed to a
detector .
24.
25. .
• Further advances such as the advent of HR- ICP-MS and ICP-TOF-
MS, during the last three decades have brought this technique to a
point where this technique can deliver detection limits of one part in
1015 for a majority of elements in the periodic table.
• Detection limits are also far below the target limits in accordance
with the analytical performance criteria described in USP 233. In
fact.
• ICP-MS is one of the two spectroscopic methods which are included
in the General chapter USP <233> for determination of elemental
impurities in pharmaceuticals.
27. Detection Limits
• ICP-MS produces the best detection limits (typically 1-10 ppt)
• Followed by GFAAS, (usually in the sub-ppb range) then ICP-AES
(of the order of 1-10 ppb) and finallyFAAS (in the sub-ppm range).
28.
29.
30. References
• V. Balaram ; Recent advances in the
determination of elemental impurities in
pharmaceuticals – Status, challenges and
moving frontiers ; Trends in Analytical
Chemistry