Hyphenated Techniques - coupling of a separation technique and an on-line spectroscopic detection technology.
Advantages of hyphenated techniques;
1. Fast and accurate analysis.
2. Higher degree of automation.
3. Higher sample throughput.
4. Better reproducibility.
5. Reduction of contamination due to its closed system.
6. Separation and quantification achieved at same time.
MASS SPECTROSCOPY ( Molecular ion, Base peak, Isotopic abundance, Metastable ...Sachin Kale
CONTENT:
Molecular Ion Peak
Significance of Molecular ion & Graphically Method
Base Peak
Isotopic Abundance
Metastable Ion
Significance of Metastable ion
Nitrogen Rule & graphs
Formulation of Rule
PRINCIPLES of FT-NMR & 13C NMR
Fourier Transform
FOURIER TRANSFORM NMR SPECTROSCOPY
THEORY OF FT-NMR
13C NMR SPECTROSCOPY
Principle
Why C13-NMR is required though we have H1-NMR?
CHARACTERISTIC FEATURES OF 13 C NMR
Chemical Shifts
NUCLEAR OVERHAUSER ENHANCEMENT
Short-Comings of 13C-NMR Spectra
MASS SPECTROSCOPY ( Molecular ion, Base peak, Isotopic abundance, Metastable ...Sachin Kale
CONTENT:
Molecular Ion Peak
Significance of Molecular ion & Graphically Method
Base Peak
Isotopic Abundance
Metastable Ion
Significance of Metastable ion
Nitrogen Rule & graphs
Formulation of Rule
PRINCIPLES of FT-NMR & 13C NMR
Fourier Transform
FOURIER TRANSFORM NMR SPECTROSCOPY
THEORY OF FT-NMR
13C NMR SPECTROSCOPY
Principle
Why C13-NMR is required though we have H1-NMR?
CHARACTERISTIC FEATURES OF 13 C NMR
Chemical Shifts
NUCLEAR OVERHAUSER ENHANCEMENT
Short-Comings of 13C-NMR Spectra
In this slide contains Interference In Atomic Absorption Spectroscopy and applications.
Presented by: Shaik Gouse ul azam. ( department of pharmaceutical analysis.)
RIPER, anantpur.
IR SPECTROSCOPY, INTRODUCTION, PRINCIPLE, THEORY, FATE OF ABSORBED RADIATION, FERMI RESONANCE, FINGERPRINT REGION, VIBRATIONS, FACTORS AFFECTING ABSORPTION OF IR RADIATION, SAMPLING TECHNIQUES, APPLICATIONS OF IR SPECTROSCOPY.
Slide covers three methods of thermal analysis i.e., thermogravimetry, differential thermal analysis, and differential scanning calorimetry. Thermal analysis methods are well-established techniques in research laboratories of pharmaceutical industry. Thermal analysis includes all methods measuring some parameter during the heating of a sample .Thermal analysis is widely used to study the thermal stability, char content, and decomposition temperature of polymer composites reinforced with natural/synthetic fibers/or nanosized fillers etc.
In this slides contains principle and instrumentation of Differential Scanning Calorimeter (DSC).
Presented by: N Poojitha. (Department of pharmaceutics),
RIPER, anantapur.
Quadrupole and Time of Flight Mass analysers.Gagangowda58
Description about important mass analysers Quadrupole and TOF: Principle, Construction and Working, Advantages and Disadvantages and their Applications.
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
In this slide contains Interference In Atomic Absorption Spectroscopy and applications.
Presented by: Shaik Gouse ul azam. ( department of pharmaceutical analysis.)
RIPER, anantpur.
IR SPECTROSCOPY, INTRODUCTION, PRINCIPLE, THEORY, FATE OF ABSORBED RADIATION, FERMI RESONANCE, FINGERPRINT REGION, VIBRATIONS, FACTORS AFFECTING ABSORPTION OF IR RADIATION, SAMPLING TECHNIQUES, APPLICATIONS OF IR SPECTROSCOPY.
Slide covers three methods of thermal analysis i.e., thermogravimetry, differential thermal analysis, and differential scanning calorimetry. Thermal analysis methods are well-established techniques in research laboratories of pharmaceutical industry. Thermal analysis includes all methods measuring some parameter during the heating of a sample .Thermal analysis is widely used to study the thermal stability, char content, and decomposition temperature of polymer composites reinforced with natural/synthetic fibers/or nanosized fillers etc.
In this slides contains principle and instrumentation of Differential Scanning Calorimeter (DSC).
Presented by: N Poojitha. (Department of pharmaceutics),
RIPER, anantapur.
Quadrupole and Time of Flight Mass analysers.Gagangowda58
Description about important mass analysers Quadrupole and TOF: Principle, Construction and Working, Advantages and Disadvantages and their Applications.
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
Gas chromatography (GC) is an analytical technique used to separate and detect the chemical components of a sample mixture to determine their presence or absence and/or quantities.Gas chromatography is usually used to separate and measure organic molecules and gases. For the technique to function, the components being analyzed must be volatile, be thermally stable, and have a molecular weight of below 1250 Da.Gas Chromatography involves the use of a separation column, which is made from a length of glass, fused silica, or metal tubing.Gas chromatography is a novel technique for separating and quantitating vaporized compounds using an inert carrier gas. It operates on similar principles to column permeation chromatography, where a sample is dissolved in a mobile phase and passed through a porous stationary structure
Gas Chromatography Thermo Fisher ScientificYuniarHasani
What is Chromatography?
Separation process that is achieved by distributing the analytes to be separated
between a mobile phase and a stationary phase.
Sample transported by mobile phase
Some components in sample interact more strongly with stationary phase
and are more strongly retained
Increasing the efficacy of drugs and at the same time reducing the chances of adverse reaction should be the aim of drug development, which can be achieved by using 3D printing to fabricate personalized medications
Drugs with narrow therapeutic index can easily be prepared using 3D printing; and, by knowing the patient’s pharmacogenetic profile and other characteristics like age, race etc., optimal dosage can be given to the patient.
3D printing technology is a valuable and potential tool for the pharmaceutical sector, leading to personalized medicine focused on the patients’ needs. It offers numerous advantages, such as increasing the cost efficiency and the manufacturing speed. 3D printing has revolutionized the way in which manufacturing is done. It improves the design manufacturing and reduces lead time and tooling cost for new products.
Nanoparticles are sub-nanosized colloidal structures composed of synthetic or semi synthetic polymers.
The drug is dissolved, entrapped, encapsulated or attached to a nanoparticle matrix.
Bioanalytical Method Development and Validation..
Bioanalytical method validation include all the procedure that demonstrate that a particular method used for quantitative measurement of analyte in given biological matrix are reliable and reproducible for intended use.
Seminar of U.V. Spectroscopy by SAMIR PANDASAMIR PANDA
Spectroscopy is a branch of science dealing the study of interaction of electromagnetic radiation with matter.
Ultraviolet-visible spectroscopy refers to absorption spectroscopy or reflect spectroscopy in the UV-VIS spectral region.
Ultraviolet-visible spectroscopy is an analytical method that can measure the amount of light received by the analyte.
(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.
Nutraceutical market, scope and growth: Herbal drug technologyLokesh Patil
As consumer awareness of health and wellness rises, the nutraceutical market—which includes goods like functional meals, drinks, and dietary supplements that provide health advantages beyond basic nutrition—is growing significantly. As healthcare expenses rise, the population ages, and people want natural and preventative health solutions more and more, this industry is increasing quickly. Further driving market expansion are product formulation innovations and the use of cutting-edge technology for customized nutrition. With its worldwide reach, the nutraceutical industry is expected to keep growing and provide significant chances for research and investment in a number of categories, including vitamins, minerals, probiotics, and herbal supplements.
Multi-source connectivity as the driver of solar wind variability in the heli...Sérgio Sacani
The ambient solar wind that flls the heliosphere originates from multiple
sources in the solar corona and is highly structured. It is often described
as high-speed, relatively homogeneous, plasma streams from coronal
holes and slow-speed, highly variable, streams whose source regions are
under debate. A key goal of ESA/NASA’s Solar Orbiter mission is to identify
solar wind sources and understand what drives the complexity seen in the
heliosphere. By combining magnetic feld modelling and spectroscopic
techniques with high-resolution observations and measurements, we show
that the solar wind variability detected in situ by Solar Orbiter in March
2022 is driven by spatio-temporal changes in the magnetic connectivity to
multiple sources in the solar atmosphere. The magnetic feld footpoints
connected to the spacecraft moved from the boundaries of a coronal hole
to one active region (12961) and then across to another region (12957). This
is refected in the in situ measurements, which show the transition from fast
to highly Alfvénic then to slow solar wind that is disrupted by the arrival of
a coronal mass ejection. Our results describe solar wind variability at 0.5 au
but are applicable to near-Earth observatories.
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.
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.
This pdf is about the Schizophrenia.
For more details visit on YouTube; @SELF-EXPLANATORY;
https://www.youtube.com/channel/UCAiarMZDNhe1A3Rnpr_WkzA/videos
Thanks...!
Deep Behavioral Phenotyping in Systems Neuroscience for Functional Atlasing a...Ana Luísa Pinho
Functional Magnetic Resonance Imaging (fMRI) provides means to characterize brain activations in response to behavior. However, cognitive neuroscience has been limited to group-level effects referring to the performance of specific tasks. To obtain the functional profile of elementary cognitive mechanisms, the combination of brain responses to many tasks is required. Yet, to date, both structural atlases and parcellation-based activations do not fully account for cognitive function and still present several limitations. Further, they do not adapt overall to individual characteristics. In this talk, I will give an account of deep-behavioral phenotyping strategies, namely data-driven methods in large task-fMRI datasets, to optimize functional brain-data collection and improve inference of effects-of-interest related to mental processes. Key to this approach is the employment of fast multi-functional paradigms rich on features that can be well parametrized and, consequently, facilitate the creation of psycho-physiological constructs to be modelled with imaging data. Particular emphasis will be given to music stimuli when studying high-order cognitive mechanisms, due to their ecological nature and quality to enable complex behavior compounded by discrete entities. I will also discuss how deep-behavioral phenotyping and individualized models applied to neuroimaging data can better account for the subject-specific organization of domain-general cognitive systems in the human brain. Finally, the accumulation of functional brain signatures brings the possibility to clarify relationships among tasks and create a univocal link between brain systems and mental functions through: (1) the development of ontologies proposing an organization of cognitive processes; and (2) brain-network taxonomies describing functional specialization. To this end, tools to improve commensurability in cognitive science are necessary, such as public repositories, ontology-based platforms and automated meta-analysis tools. I will thus discuss some brain-atlasing resources currently under development, and their applicability in cognitive as well as clinical neuroscience.
Body fluids_tonicity_dehydration_hypovolemia_hypervolemia.pptx
Hyphenated techniques- GCMS, LCMS, GCIR
1. Presented By :
Mr. Sanket Rajiv Shinde
M. Pharmacy (QAT)
Savitribai Phule Pune University
2. Contents
1. Introduction
2. List of Hyphenated Techniques
3. GC-MS
4. LC-MS
5. GC-IR
6. LC-ESI-MS
7. Advantages of Hyphenated Techniques
8. References
2
3. What Is Hyphenated Technique ?(1)
The term “hyphenation” was first adapted by Hirschfeld in
1980.
The technique developed from the coupling of a separation
technique and an on-line spectroscopic detection technology
is known as hyphenated technique.
3
Introduction
7. Principles :
GC :
• May be Gas Liquid [GLC] or Gas Solid Chromatography [GSC]
but GLC is preferred
• GLC works by partition but GSC works by adsorption
• In GLC the substance to be studied first converted to gas which
works as the mobile phase.
MS :
1. Ion Formation
2. Ion Separation & Detection 7
GC-MS conti….
8. • Techniques used to form ions are:
1. Electron Ionisation
2. Chemical Ionisation
3. Desorption Ionisation
i. Secondary Ion Mass Spectroscopy [SIMS]
ii. Fast Atom Bombardment [FAB]
iii. Matrix Associated Laser Desorption
Ionisation [MALDI]
4. Electrospray Ionisation
8
1. Ion Formation
GC-MS conti….
9. 2. Ion Separation and Detection
• Types of instruments are used:
i. Direct Focusing Type:
a) Single Focusing
b) Double Focusing
ii. Quadruple Mass Analyser
iii. Quadruple Mass Storage
iv. Time of Flight Mass Analyser
9
GC-MS conti….
10. Instrumentation of GC :
A. Carrier Gas:
• Chemically inert
• Suitable for the detector use
• Amount of impurity should be less
• Easily available and should be cheap
• Non inflammable
Generally used carrier gases are
He, H, N, Ar etc.
10
GC-MS conti….
11. B. Flow Regulators:
Used to maintain the
uniform pressure and
flow rate.
Generally used are:
• Rotameter
• Soap Bubble Flow Meter
11
GC-MS conti….
12. C. Injection Devices:
• GAS : Valve Devices
• LIQUID : Loop Devices
• SOLID : Dissolve the
substance in suitable
solvent and then inject.
12
GC-MS conti….
13. D. Columns:
Columns can be of the following types:
• Packed Columns [Stationary Phase- PEG]
• Open Tubular Column or Open Capillary Column/ GOLAY Column
• SCOT ( Support Coated Open Tubular Column)
13
GC-MS conti….
14. E. Temperature Controlling Devices:
The devices are very important role playing.
Generally used Temperature Controlling Devices are:
• Pre heaters(for vapour formation)
• Thermostatically controlled oven
14
GC-MS conti….
16. Principle of working and interfaces :
GC-MS works by :
1. Iso Thermal Principle
2. Liner Principle
Interfaces of GC MS are :
1. Molecular Separator
2. Permeation Separator
3. Open Split
4. Capillary Direct
16
GC-MS conti….
18. Gather Evidence
18
Police Officer
1. Interview witness
2. Dust for fingerprints
Mass Spectrometrist
1. Interview biologists who
isolated the protein
2. Cleave protein to obtain
peptide mixture
3. Analyse peptide mixture by MS
to obtain Peptide molecular
masses !
GC-MS conti….
19. 19
Database Search Results
Police Officer
Identifies the robber
Mr. XYZ
Mass Spectrometrist
Identifies the protein
e.g. bovine carbonic
anhydrase
GC-MS conti….
20. Applications of GC-MS :(1)
Elucidation of the structure of organic & biological
molecules.
Impurity profiling of pharmaceuticals.
Identification of components in thin layer & paper
chromatograms.
Identification of drugs of abuse & metabolites of drugs of
abuse in blood, urine & saliva.
20
GC-MS conti….
21. Sports antidoping analysis (in forensic GC-MS).
Analyzer of aerosol particles.
Determination of pesticide residues in food.
Polymer characterization (pyrolysis methods combined
GCMS).
Drug monitoring & toxicology studies.
Explosive analysis
Environmental analysis
21
GC-MS conti….
35. Detectors :
Records either the charge induced or the current produced
when an ion passes by or hits a surface.
A continuous dynode particle
multiplier detector
35
LC-MS conti….
39. Pharmacokinetics: Bio analysis
Drug development
Molecular weight determination
Toxicology
Impurity detection
Determination of isotopes
Proteomics/Metabolomics
Determination of pesticides, herbicides & organic
pollutants for environmental ,monitoring.
Applications of LC-MS :(1)
39
LC-MS conti….
40. Comparison of LC-MS with GC-MS :
• GC-MS requires compounds to be volatile to be ionised.
- traditionally electron impact source is used.
• LC-MS can be used to detect compounds from poly-
aromatic (non-polar) to peptide & proteins.
• GC-MS is still able to detect long chain aliphatic
compounds (petroleum based analytes) & very low mass
volatile material better than LC-MS.
40
41. Very sensitive, very expensive, sample recovery is also
possible because IR is non-destructive technique.
In this, GC does the separation part where as IR perform
function of identification.
Effluent from GC is directly forwarded into the heated
pipe of IR at atmospheric pressure.
IR spectroscopy identifies the compound by identifying
the functional group. 41
GC-IR
Gas
Chromatography
Infrared
Spectroscopy
GC-IR
42. 42
Applications of GC-IR :
DNA analysis of blood samples, other fluids.
Pharmaceutical applications
Industrial applications
GC-IR conti….
45. 1. Fast and accurate analysis.
2. Higher degree of automation.
3. Higher sample throughput.
4. Better reproducibility.
5. Reduction of contamination due to its closed system.
6. Separation and quantification achieved at same time.
45
Advantages of
Hyphenated Techniques:
46. 1. Kalpesh N Patel, et al ; Introduction to hyphenated techniques and their
applications in Pharmacy; Pharmaceutical Methods; Oct-Dec 2010; Vol 1 ;
Issue 1.
2. Silverstein R; Spectroscopic Identification of Organic Compounds; Wiley
Publication Delhi; 6th edition; 2009; Page 2-70
3. Skoog D et al; Fundamentals of Analytical Chemistry; Cengage Brain
Publication London; 9th edition; 2010; Page 16-25.
4. AH Beckett, J.B Stenlake, Pharmaceutical chemistry;4th edition-Part
2;Page 474-477.
5. Gurdeep R. Chatwal, K. Anand; Instrumental methods of chemical
analysis; Page 2.272,2.673
6. G. C. Stafford et al.; International Journal of Mass Spectrometry and Ion
Processes, 60; 1984, Page 85 and Analytical Chemistry, 59; 1987, Page
1677.
7. https://www.jic.ac.uk/services/metabolomics/topics/lcms/why.htm
46
References