• It is the combination of liquid chromatography and the mass spectrometry.
• Liquid chromatography-mass spectrometry (LC-MS) is an analytical chemistry
technique that combines the physical separation capabilities of liquid
chromatography with the mass analysis capabilities of mass spectrometry.
• The combination of these two powerful techniques gives the chemical analyst the
ability to analyze virtually any molecular species; including, thermally labile, non
volatile, and high molecular weight species.
this will help to know about the advance technique to analysis the biological sample in cancer diagnosis and general separation of proteins based upon the molecular weight and helps to analysis the new drug synthesis level
GCMS & LCMS
htps://youtube.com/vishalshelke99
https://instagram.com/vishal_stagram
Sub :- Advanced Analytical Techniques
M.Pharmacy Sem1
Savitribai Phule Pune University
Contents :-
GC-MS
Introduction
Principle
Instrumentation
Application
LC-MS
Introduction
Principle
Instrumentation
Application
Introduction to Gas chromatography-Mass spectroscopy
Gas chromatography-Mass spectroscopy is one of the so-called hyphenated analytical techniques. It is actually two techniques that are combined to form a single method of analyzing mixtures of chemicals
GC-MS is an instrumental technique, comprising a gas chromatograph coupled to a mass spectrometer by which complex mixtures of chemicals may be separated, identified & quantified. In order to a compound to be analysed by GC-MS it must be sufficiently volatile & thermally stable.
Principle :-
The Sample solution is injected into the GC inlet where it is vapourized & swept onto a chromatographic column by the carrier gas ( usually helium). The sample flows through the column & compounds comprising the mixture of interest are separated by virtue of their relative interaction with the coating of the column (stationery phase) & the carrier gas (mobile phase). The later part of the column passes through a heated transfer line & ends at the entrance to ion source where compounds eluting from the column are converted to ions
various parts of mAss spectroscopy, applications, principle, peaks, rules, typical mass spectra, various combinations, Fragmentation, rules of fragmentation and useful points which can help Chemical and analytical students and structural elucidation.
GAS CHROMATOGRAPHY-MASS SPECTROSCOPY [GC-MS]Shikha Popali
THIS PRESENTATION GIVES A DETAIL ACCOUNT ON THE GC-MS WITH ITS INTRODUCTION, BASIC PRINCIPLE OF BOTH COMBINED AND INDIVIDUALLY WITH ITS INSTRUMENTATION, APPLICATION AND EXAMPLES, MAKES EASY TO COLLECT ALL THE DATA AT A PLACE ACCORDING TO THE M.PHARM SYLLABUS S PER PCI
• It is the combination of liquid chromatography and the mass spectrometry.
• Liquid chromatography-mass spectrometry (LC-MS) is an analytical chemistry
technique that combines the physical separation capabilities of liquid
chromatography with the mass analysis capabilities of mass spectrometry.
• The combination of these two powerful techniques gives the chemical analyst the
ability to analyze virtually any molecular species; including, thermally labile, non
volatile, and high molecular weight species.
this will help to know about the advance technique to analysis the biological sample in cancer diagnosis and general separation of proteins based upon the molecular weight and helps to analysis the new drug synthesis level
GCMS & LCMS
htps://youtube.com/vishalshelke99
https://instagram.com/vishal_stagram
Sub :- Advanced Analytical Techniques
M.Pharmacy Sem1
Savitribai Phule Pune University
Contents :-
GC-MS
Introduction
Principle
Instrumentation
Application
LC-MS
Introduction
Principle
Instrumentation
Application
Introduction to Gas chromatography-Mass spectroscopy
Gas chromatography-Mass spectroscopy is one of the so-called hyphenated analytical techniques. It is actually two techniques that are combined to form a single method of analyzing mixtures of chemicals
GC-MS is an instrumental technique, comprising a gas chromatograph coupled to a mass spectrometer by which complex mixtures of chemicals may be separated, identified & quantified. In order to a compound to be analysed by GC-MS it must be sufficiently volatile & thermally stable.
Principle :-
The Sample solution is injected into the GC inlet where it is vapourized & swept onto a chromatographic column by the carrier gas ( usually helium). The sample flows through the column & compounds comprising the mixture of interest are separated by virtue of their relative interaction with the coating of the column (stationery phase) & the carrier gas (mobile phase). The later part of the column passes through a heated transfer line & ends at the entrance to ion source where compounds eluting from the column are converted to ions
various parts of mAss spectroscopy, applications, principle, peaks, rules, typical mass spectra, various combinations, Fragmentation, rules of fragmentation and useful points which can help Chemical and analytical students and structural elucidation.
GAS CHROMATOGRAPHY-MASS SPECTROSCOPY [GC-MS]Shikha Popali
THIS PRESENTATION GIVES A DETAIL ACCOUNT ON THE GC-MS WITH ITS INTRODUCTION, BASIC PRINCIPLE OF BOTH COMBINED AND INDIVIDUALLY WITH ITS INSTRUMENTATION, APPLICATION AND EXAMPLES, MAKES EASY TO COLLECT ALL THE DATA AT A PLACE ACCORDING TO THE M.PHARM SYLLABUS S PER PCI
Hyphenated technique is a combination or coupling of two analytical techniques with the help of proper interface.
In this presentation Hyphenated techniques-LC-MS/MS, GC-MS/MS, HPTLC-MS has been discussed
The aim of the coupling is to obtain an information-rich detection for both identification and quantification compared to that with a single analytical technique.
LC/MS is a technique that combines physical separation capabilities of LC with mass analysis capability of MS.
It is a method that combines separation power of HPLC with detection power of MS.
In LC-MS we remove the detector from the column of LC and fit the column to interface of MS.
In the most of the cases the interface used in LC-MS are ionization source.
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
MUTUAL PRODRUG IS DISCUSSED HERE IN DETAIL WITH ITS MULTIPLE TYPES AND FUCTIONAL GROUPS IT IS USE FOR AND FAILURE WITH PRODRUGS, WITH PHARMACEUTICAL EXAMPLES AND STRUCTURE ARE ALSO SHARE, SYNTHETIC APLLICATIONS.
HERE PRESENTS AN OLIGONUCLEOTIDE THERAPY, ITS INTRODUCTION TO OLIGONUCLEOTIDE, ITS TECHNIQUES, DEVELOPED METHODS AND THEIR APP,LICATIONS IN PHARMACEUTICAL ARE HERE DISCUSSED IN DETAIL
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SYNTHETIC REAGENTS AND APPLICATIONS OF ALUMINIUM ISOPROPOXIDE ITS ALTERNATIVE NAMES AND ITS PHYSICAL PROPERTIRS , HANDLING, STORAGE, PRECAUTIONS, PREPARATIONS, SYNTHETIC APPLICATIONS
PTC IS THE PHASE TRANSFER CATALYSIS HERE TYPES OF PTC ARE DISCUSSED , THEORIES OF CATALYSIS AND MECHANISM OF PTC, ADVANTAGES OF PTC, APPLICATION OF PTC
SWERTIA CHIRATA NATURAL PRODUCT OF PHARMACEUTICALSShikha Popali
HERE THE NATURAL PRODUCT SERTIA CHIRATA IS DISCUSSED WITH ITS COMMON NAME, CHEMICAL CONSTITUENTS, ACTIVE CONSTITUENTS, SAR, MEDICINAL ACTIVITY AND MORE
THE DCC I.E. DICYCLOCARBODIIMDE IS A REAGENT AND HERE THE DETAIL ACCOUNT ON IT IS GIVEN INCLUDING MOLECULAR WEIGHT, STRUCTURE, SYNTHESIS AND PHYSICAL PARAMETERS AND APPLICATIONS FOR OTERS SYNTHESIS ARE ALSO DISCUSSED, THE DIFFERENT SYNTHESIS WITH DCC COMBINATION ARE ALSO MENTIONED
COMPARATIVE EVALUATION OF DIFFERENT PARACETAMOL BRANDSShikha Popali
THE PARACETAMOL TABLETS IS COMMONLY TAKEN AND PRESCRIBED FOR FEVER , SO HERE WE HAVE MADE PRACTICAL IS IT TRUE EVALUATION LABEL AND WHICH BRAND IS MORE SAFE.
Palestine last event orientationfvgnh .pptxRaedMohamed3
An EFL lesson about the current events in Palestine. It is intended to be for intermediate students who wish to increase their listening skills through a short lesson in power point.
How to Make a Field invisible in Odoo 17Celine George
It is possible to hide or invisible some fields in odoo. Commonly using “invisible” attribute in the field definition to invisible the fields. This slide will show how to make a field invisible in odoo 17.
The French Revolution, which began in 1789, was a period of radical social and political upheaval in France. It marked the decline of absolute monarchies, the rise of secular and democratic republics, and the eventual rise of Napoleon Bonaparte. This revolutionary period is crucial in understanding the transition from feudalism to modernity in Europe.
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This slides describes the basic concepts of ICT, basics of Email, Emerging Technology and Digital Initiatives in Education. This presentations aligns with the UGC Paper I syllabus.
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Synthetic fiber production is a fascinating and complex field that blends chemistry, engineering, and environmental science. By understanding these aspects, students can gain a comprehensive view of synthetic fiber production, its impact on society and the environment, and the potential for future innovations. Synthetic fibers play a crucial role in modern society, impacting various aspects of daily life, industry, and the environment. ynthetic fibers are integral to modern life, offering a range of benefits from cost-effectiveness and versatility to innovative applications and performance characteristics. While they pose environmental challenges, ongoing research and development aim to create more sustainable and eco-friendly alternatives. Understanding the importance of synthetic fibers helps in appreciating their role in the economy, industry, and daily life, while also emphasizing the need for sustainable practices and innovation.
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He discussed the concept of quality improvement, emphasizing its applicability to various aspects of life, including personal, project, and program improvements. He defined quality as doing the right thing at the right time in the right way to achieve the best possible results and discussed the concept of the "gap" between what we know and what we do, and how this gap represents the areas we need to improve. He explained the scientific approach to quality improvement, which involves systematic performance analysis, testing and learning, and implementing change ideas. He also highlighted the importance of client focus and a team approach to quality improvement.
2. Principle:
• LC/MS is a technique that combines physical separation
capabilities of liquid chromatography with mass analysis
capabilityofMassspectrometry.
• ItisamethodthatcombinesseparationpowerofHPLCwith
detectionpowerofMassspectrometry.
• InLC-MSweremovethedetectorfromthecolumnofLCandfit the
columntointerfaceofMS.
• InthemostofthecasestheinterfaceusedinLC-MSareionization source.
INTRODUCTION
3. • HPLCisamethod for separatingacomplexmixture in to its
components.
• Highsensitivityof massspectroscopy provides theinformation
for identification of compoundsor structural elucidation of
compounds.
• Combination of thesetwotechniques isLC-MS.
• Asthe metabolitesappearfrom the endof the column they
enter the massdetector, where the solvent isremovedand the
metabolitesareionized.
Theory of LC/MS
4. LC-MS System Components
• Mass spectrometers work by ionizing molecules and then
sorting and identifying the ions according to their mass-
to-charge (m/z) ratios.
5. HPLC
• Liquidphaseoperation
• 25- 50deg.C
• Nomassrange
limitations
• Inorganicbuffers
• 1ml/min eluent flowis
equivalent to 500 ml/min
ofgas
MS
• Vacuumoperation
200- 300deg.C
• Upto 4000Dafor
quadrupole MS
• Requiresvolatile
buffers
• Accepts10ml/min gas
flow
PROBLEMS IN COMBINING HPLC AND MS
6. Themobile phaseisthe solvent that movesthe solute throughout
column.
Generalrequirements:-
(1) Lowcost,UVtransparency,high purity.
(2) Lowviscosity,low toxicity, nonflammability.
(3) Noncorrosiveto LCsystemcomponent.
Solventstrength andselectivity:-
It isthe abilityof solvent to elute solutesfromacolumn.
MOBILE PHASE
7. • The use of di-functional or tri-functional silanes to create bonded
groups with two or three attachment points leading to phases
with higher stability in low or higher pHandlower bleedfor LC-MS
• Most widely usedcolumnsfor LC-MSare :-
(1) fast LC column :-
the useof short column.(15-50mm)
(2) Micro LC column :-
the useof largecolumn. (20-150mm)
COLUMN
8. • Samplepreparation generally consists of concentrating the analyte
and removing compounds that can cause background ion or
suppressionization.
• Exampleof samplepreparationinclude:-
• OnColumnconcentration -to increaseanalyteconcentration.
• Desalting - to reduce the sodium and potassium adduct
formation that commonlyoccursin electrospray.
• Filtration- to separate a low molecular-weight drug from
proteins in plasma,milk, ortissue.
Sample preparation
9. • LC-MSsystemsinclude adevicefor introducing samples(suchas an
HPLC)aninterface for connectingsuchdevice,anion source that
ionizessamples,anelectrostatic lensthat efficiently introduces
the generatedions, amassanalyzerunit that separatesions based
on their mass-to-charge(m/z) ratio, anda detector unit that
detectstheseparatedions.
• In anLC-MSsystem,however, if the LCunit issimplyconnected
directlyto the MSunit, the liquid mobile phasewould vaporize,
resulting in large amountsof gasbeingintroduced into the MS
unit.
• Thiswould decreasethe vacuumlevel andprevent the targetions
from reachingthe detector. Sointerfaces are tobeused.
INTERFACES
10. • It isdifficult to interface aliquid chromatographyto amass-
spectrometercauseof the necessityto removethe solvent.
• Thecommonlyusedinterfacesare:-
(1) Electrosprayionization(ESI)
(2) Thermosprayionization(TSI)
(3) Atmosphericpressurechemicalionization(APCI)
(4) Atmosphericpressurephotoionization(APPI)
TYPES OF INTERFACES
11. • ESIdrawssamplesolutions to the tip of acapillarytube,
whereit appliesahighvoltage of about 3to 5kV.
• A nebulizer gas flows from outside the capillary to spray the
sample.Thiscreatesafine mist of chargeddroplets with the same
polarity asthe appliedvoltage.
• Asthischargedparticles move,the solvent continuesto evaporate,
thereby increasingthe electricfield onthe droplet surface.When
the mutual repulsive force of the charges exceedsthe liquid
surfacetension, then fissionoccurs.
• Asthis evaporation andfissioncycleisrepeated, thedroplets
eventually becomesmallenoughthat the sampleionsare
liberated into the gasphase.
ElectroSprayIonization(ESI)
12. • ESIprovides the softest ionization method available, which
meansit canbeusedfor highly polar, least volatile, or
thermally unstablecompounds.
ElectroSprayIonization(ESI)
14. • Theyareof 2type:
• a)Real-TSPionization
• b) Dischargeelectrode for external ionizationandrepeller
electrode
Thermospray ionization (TSI)
15. • TheLC eluent isvaporizedusingaheater at atmospheric pressure.
Theresulting gas ismadeto pass through a beamof photons
generated byadischargelamp(UVlamp) which ionizesthe gas
molecules.
Atmospheric pressurephotoionization(APPI)
16. • Theydeflect ionsdown acurvedtubes in amagnetic fields based
on theirkinetic energydetermined bythe mass,charge and
velocity.
• Themagnetic field isscannedto measuredifferentions.
• Typesof massanalyzer:-
(1) Quadrapolemassfilter.
(2) Timeof flight
(3) Iontrap
(4) Fourier transform ion cyclotron resonance(FT-ICR)
Mass Analyser
17. • A Quadrupolemassfilter consistsof four parallelmetal rodswith different
charges
• Twooppositerodshaveanapplied +potential andthe othertwo
rodshavea-potential
• Theappliedvoltages affect the trajectory of ionstravelingdown the flight
path
• ForgivenDC andAC voltages,only ionsof acertain mass-to-charge ratio pass
through the quadrupole filter and all other ionsare thrownout of their
originalpath.
QuadrupoleMassAnalyzer
18. • TOFAnalyzersseparateionsbytime without the useofan
electric or magneticfield.
• In acrude sense,TOF issimilar to chromatography, except there is
no stationary/ mobile phase,insteadtheseparationis basedon
the kineticenergyandvelocityof the ions.
TOF (Time of Flight)Mass Analyzer
19. • It usesanelectricfield for the separationof the ionbymass to
chargeratios.
• Theelectricfield in the cavitydueto the electrodescauses the
ionsof certainm/z valuesto orbit in the space.
Ion TrapMass Analyzer
20. • Usesamagneticfield in orderto trap ionsinto anor bit inside of it.
• Inthisanalyzerthereisnoseparationthat occursrather all the
ionsof aparticular rangearetrapped inside,andan applied
external electric field helpstogenerate asignal.
Fourier Transform ion cyclotron
resonance (FT-ICR)
21. PharmaceuticalApplications:
Rapidchromatographyofbenzodiazepines
Identificationofbileacidmetabolite
BiochemicalApplications:
Rapid protein identification using capillary LC/MS/MS and
databasesearching.
ClinicalApplications:
High-sensitivitydetectionoftrimipramineandthioridazine
Applications of LC-MS