This ppt explains the basics of mass spectrometry and in application in pharmacognosy. Hope this helps you guys. Like, comment and save. If you hav problem downloading, send your email address; i'll post it for you by mail :)
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a substance can absorb any visible light or external radiation and then again emit it. this called fluorescence and the process of reduction in fluorescence intensity is called quenching. this presentation is all about quenching of fluorescence.
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.
a substance can absorb any visible light or external radiation and then again emit it. this called fluorescence and the process of reduction in fluorescence intensity is called quenching. this presentation is all about quenching of fluorescence.
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.
In this slide contains principle, instrumentation, methodology, and application of gel chromatography.
Presented by: SATHEES CHANDRA (Department of pharmaceutical analysis).
RIPER, anantapur
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
Presenting a topic which is entitled: Detectors
Above topic includes:
Types of detector
phototube detector
photomultiplier tubes
silicon photodiodes
photovoltaic cells
advantages
multi-channel photon detectors
linear photodiode arrays
photodiode array
with basics of instrumentation and science technology
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Thanking-You
Preeti Choudhary
Polarographic technique is applied for the qualitative or quantitative analysis of electroreducible or oxidisable elements or groups.
It is an electromechanical technique of analyzing solutions that measures the current flowing between two electrodes in the solution as well as the gradually increasing applied voltage to determine respectively the concentration of a solute and its nature.
The principle in polarography is that a gradually increasing negative potential (voltage) is applied between a polarisable and non-polarisable electrode and the corresponding current is recorded.
Polarisable electrode: Dropping Mercury electrode
Non-polarisable electrode: Saturated Calomel electrode
From the current-voltage curve (Sigmoid shape), qualitative and quantitative analysis can be performed. This technique is called as polarography, the instrument used is called as polarograph and the current-voltage curve recorded is called as polarogram
In this slide contains principle, instrumentation, methodology, and application of gel chromatography.
Presented by: SATHEES CHANDRA (Department of pharmaceutical analysis).
RIPER, anantapur
Introduction
working principle
fragmentation process
general rules for fragmentation
general modes of fragmentation
metastable ions
isotopic peaks
applications
Presenting a topic which is entitled: Detectors
Above topic includes:
Types of detector
phototube detector
photomultiplier tubes
silicon photodiodes
photovoltaic cells
advantages
multi-channel photon detectors
linear photodiode arrays
photodiode array
with basics of instrumentation and science technology
https://www.linkedin.com/in/preeti-choudhary-266414182/
https://www.instagram.com/chaudharypreeti1997/
https://www.facebook.com/profile.php?id=100013419194533
https://twitter.com/preetic27018281
Please like, share, comment and follow.
stay connected
If any query then contact:
chaudharypreeti1997@gmail.com
Thanking-You
Preeti Choudhary
Polarographic technique is applied for the qualitative or quantitative analysis of electroreducible or oxidisable elements or groups.
It is an electromechanical technique of analyzing solutions that measures the current flowing between two electrodes in the solution as well as the gradually increasing applied voltage to determine respectively the concentration of a solute and its nature.
The principle in polarography is that a gradually increasing negative potential (voltage) is applied between a polarisable and non-polarisable electrode and the corresponding current is recorded.
Polarisable electrode: Dropping Mercury electrode
Non-polarisable electrode: Saturated Calomel electrode
From the current-voltage curve (Sigmoid shape), qualitative and quantitative analysis can be performed. This technique is called as polarography, the instrument used is called as polarograph and the current-voltage curve recorded is called as polarogram
(MS) is an analytical technique that produces spectra (singular spectrum) of the masses of the atoms or molecules comprising a sample of material. The spectra are used to determine the elemental or isotopic signature of a sample, the masses of particles and of molecules, and to elucidate the chemical structures of molecules, such as peptides and other chemical compounds,so it is considered one f the very important diagnostic analytical techniques .
BITS - Introduction to Mass Spec data generationBITS
This is the first presentation of the BITS training on 'Mass spec data processing'.
It reviews the basic concepts of mass spectrometry data generation.
Thanks to the Compomics Lab of the VIB for contribution.
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
Quantitative Analysis of 30 Drugs in Whole Blood by SPE and UHPLC-TOF-MSAnnex Publishers
Abstract
An Ultra-High Pressure Liquid Chromatography Time-of-Flight Mass Spectrometry (UHPLC-TOF-MS) method for quantitative analysis of 30 drugs in whole blood was developed and validated. The method was used for screening and quantification of common drugs and drugs of abuse in whole blood received from autopsy cases and living persons. The compounds included: alprazolam, amphetamine, benzoylecgonine, bromazepam, cathine, cathinone, chlordiazepoxide, cocaine, codeine, clonazepam, 7-aminoclonazepam, diazepam, nordiazepam, flunitrazepam, 7-aminoflunitrazepam, ketamine, ketobemidone, 3,4-Methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), methamphetamine, methadone, morphine, 6-monoacetylmorphine, nitrazepam, 7-aminonitrazepam, oxazepam, temazepam, tramadol, O-desmethyltramadol, and zolpidem. Blood samples (200 μL) were subjected to Solid Phase Extraction (SPE). Target drugs were quantified using a Waters ACQUITY UPLC system coupled to a Waters SYNAPT G2 TOF-MS apparatus. Extraction recoveries ranged from 41% (7-aminoclonazepam) to 111% (ketamine) and matrix effects ranged from -13% (temazepam) to 50% (7-aminonitrazepam). For all compounds, a quadratic polynomial was applied for fitting the calibration curves. Lower Limits of Quantification (LOQ) ranged from 0.005 to 0.05 mg/kg. Satisfactory precisions below 15% and accuracies within 85-115% were obtained for all compounds at concentrations exceeding the LOQ. In conclusion, we present a validated UHPLC-TOF-MS method for simultaneous quantification of 30 drugs in whole blood with a run time of 15 min using 200 μL of whole blood.
Keywords: Drugs of abuse, UHPLC-TOF-MS, Whole blood, SPE, Quantification
Toxicological Screening and Quantitation Using Liquid Chromatography/Time-of-...Annex Publishers
In recent years, an increasing number of new designer-drugs have increased the demands for general toxicological screening [1]. Limited screening based on immunoassays is commonly used in clinical toxicology, whereas more comprehensive approaches are common in forensic toxicology such as screening based on Gas or Liquid Chromatography (GC or LC) approaches [2]. The classic approach has been gas chromatography-Mass Spectrometry (GC-MS) combined with LC-diode-array detection (DAD) for systematic toxicological analysis. This setup has the advantage of covering a very broad spectrum of drugs and illicit substances when combined with library search facilities. However, the analytical sensitivity and specificity of LC-DAD may not be optimal. Thus, more sensitive and specific screening techniques based exclusively on LC combined with mass spectrometry have gained popularity. Multi-target screening and quantitation methods based on LC-tandem mass spectrometry (MS/MS) may provide detection of hundred or more compounds [3]. Using ion-trap MSn detection, several hundred compounds can be detected [4]. A more extended screening is possible using time-of-flight (TOF) mass spectrometry, which is a high-resolution mass spectrometry technique that detects drugs on the basis of their exact mass. Using this technique, scanning is performed over all masses for low molecular drugs, and detected signals can be related to a library of exact drug masses. Retention time and fragmentation pattern contribute to the identification. In principle, it is possible to screen for thousands of compounds, although issues related to software capabilities may limit the number of compounds to several hundred in daily practice [5-7].
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
This ppt was made by my friend Svenia & I. It is a summary of the journal on 'Influence of mineral and vitamin supplements on pregnancy outcome'.
Hope it helps.
This is a summary of the journal : 'Is there more to learn about functional vitamin D metabolism?' presented by my friend Svenia and me. Hope it helps.
This presentation is on ocean acidification, it covers
(1) a background on ocean acidification,
(2) the chemistry between carbon dioxide & the ocean
(3) Impact of Ocean acidification on biological processes and the ecosystems.
(4) and finally some mitigation measures
I hope this ppt be useful & helpful to people working on this topic :)
Enjoy
This is a portfolio on 5 different plants with pharmacological properties prepared by my colleague Svenia and Myself. It covers some important aspects such as background, uses and preparations etc. Hope it helps.
Gap junctional intercellular communication in cancer chemopreventionNabiilah Naraino Majie
This powerpoint presentation gives an overview of how gap junctions are involved in cancer. And how it can be upregulated by the action of phytochemicals in the process of cancer chemoprevention. I have used a scientific journal to eleborate on the mechanism. I hope it helps.
This presentation is on the bioassay of heparin which helps to know the potency of new heparin drug or heparin conc in individual suffering from heparin resistance diseases.
This was made by my friend Naailah and me. Hope it helps.
This prsentation explains the use of biomarker with reference to an article: Accelerating Drug Develeopment using Biomarkers-Sitagliptin.
It was presented my my 2 friends and me. Hope it helps you guys.
A presentation on Paul Ehrlich developed modern chemotherapy. This was my ppt for the module pharmaceutics 6. It i based on Anti microbial chemo; hope it help others doing relating things.
This was my pharmaceutics presentation for mixing. Provides definitions, mechanism, types of mixers etc.
P.S: I am not the sole presenter. Ideas are from my two other colleagues as well.
NVBDCP.pptx Nation vector borne disease control programSapna Thakur
NVBDCP was launched in 2003-2004 . Vector-Borne Disease: Disease that results from an infection transmitted to humans and other animals by blood-feeding arthropods, such as mosquitoes, ticks, and fleas. Examples of vector-borne diseases include Dengue fever, West Nile Virus, Lyme disease, and malaria.
Ethanol (CH3CH2OH), or beverage alcohol, is a two-carbon alcohol
that is rapidly distributed in the body and brain. Ethanol alters many
neurochemical systems and has rewarding and addictive properties. It
is the oldest recreational drug and likely contributes to more morbidity,
mortality, and public health costs than all illicit drugs combined. The
5th edition of the Diagnostic and Statistical Manual of Mental Disorders
(DSM-5) integrates alcohol abuse and alcohol dependence into a single
disorder called alcohol use disorder (AUD), with mild, moderate,
and severe subclassifications (American Psychiatric Association, 2013).
In the DSM-5, all types of substance abuse and dependence have been
combined into a single substance use disorder (SUD) on a continuum
from mild to severe. A diagnosis of AUD requires that at least two of
the 11 DSM-5 behaviors be present within a 12-month period (mild
AUD: 2–3 criteria; moderate AUD: 4–5 criteria; severe AUD: 6–11 criteria).
The four main behavioral effects of AUD are impaired control over
drinking, negative social consequences, risky use, and altered physiological
effects (tolerance, withdrawal). This chapter presents an overview
of the prevalence and harmful consequences of AUD in the U.S.,
the systemic nature of the disease, neurocircuitry and stages of AUD,
comorbidities, fetal alcohol spectrum disorders, genetic risk factors, and
pharmacotherapies for AUD.
Report Back from SGO 2024: What’s the Latest in Cervical Cancer?bkling
Are you curious about what’s new in cervical cancer research or unsure what the findings mean? Join Dr. Emily Ko, a gynecologic oncologist at Penn Medicine, to learn about the latest updates from the Society of Gynecologic Oncology (SGO) 2024 Annual Meeting on Women’s Cancer. Dr. Ko will discuss what the research presented at the conference means for you and answer your questions about the new developments.
Acute scrotum is a general term referring to an emergency condition affecting the contents or the wall of the scrotum.
There are a number of conditions that present acutely, predominantly with pain and/or swelling
A careful and detailed history and examination, and in some cases, investigations allow differentiation between these diagnoses. A prompt diagnosis is essential as the patient may require urgent surgical intervention
Testicular torsion refers to twisting of the spermatic cord, causing ischaemia of the testicle.
Testicular torsion results from inadequate fixation of the testis to the tunica vaginalis producing ischemia from reduced arterial inflow and venous outflow obstruction.
The prevalence of testicular torsion in adult patients hospitalized with acute scrotal pain is approximately 25 to 50 percent
Lung Cancer: Artificial Intelligence, Synergetics, Complex System Analysis, S...Oleg Kshivets
RESULTS: Overall life span (LS) was 2252.1±1742.5 days and cumulative 5-year survival (5YS) reached 73.2%, 10 years – 64.8%, 20 years – 42.5%. 513 LCP lived more than 5 years (LS=3124.6±1525.6 days), 148 LCP – more than 10 years (LS=5054.4±1504.1 days).199 LCP died because of LC (LS=562.7±374.5 days). 5YS of LCP after bi/lobectomies was significantly superior in comparison with LCP after pneumonectomies (78.1% vs.63.7%, P=0.00001 by log-rank test). AT significantly improved 5YS (66.3% vs. 34.8%) (P=0.00000 by log-rank test) only for LCP with N1-2. Cox modeling displayed that 5YS of LCP significantly depended on: phase transition (PT) early-invasive LC in terms of synergetics, PT N0—N12, cell ratio factors (ratio between cancer cells- CC and blood cells subpopulations), G1-3, histology, glucose, AT, blood cell circuit, prothrombin index, heparin tolerance, recalcification time (P=0.000-0.038). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and PT early-invasive LC (rank=1), PT N0—N12 (rank=2), thrombocytes/CC (3), erythrocytes/CC (4), eosinophils/CC (5), healthy cells/CC (6), lymphocytes/CC (7), segmented neutrophils/CC (8), stick neutrophils/CC (9), monocytes/CC (10); leucocytes/CC (11). Correct prediction of 5YS was 100% by neural networks computing (area under ROC curve=1.0; error=0.0).
CONCLUSIONS: 5YS of LCP after radical procedures significantly depended on: 1) PT early-invasive cancer; 2) PT N0--N12; 3) cell ratio factors; 4) blood cell circuit; 5) biochemical factors; 6) hemostasis system; 7) AT; 8) LC characteristics; 9) LC cell dynamics; 10) surgery type: lobectomy/pneumonectomy; 11) anthropometric data. Optimal diagnosis and treatment strategies for LC are: 1) screening and early detection of LC; 2) availability of experienced thoracic surgeons because of complexity of radical procedures; 3) aggressive en block surgery and adequate lymph node dissection for completeness; 4) precise prediction; 5) adjuvant chemoimmunoradiotherapy for LCP with unfavorable prognosis.
Recomendações da OMS sobre cuidados maternos e neonatais para uma experiência pós-natal positiva.
Em consonância com os ODS – Objetivos do Desenvolvimento Sustentável e a Estratégia Global para a Saúde das Mulheres, Crianças e Adolescentes, e aplicando uma abordagem baseada nos direitos humanos, os esforços de cuidados pós-natais devem expandir-se para além da cobertura e da simples sobrevivência, de modo a incluir cuidados de qualidade.
Estas diretrizes visam melhorar a qualidade dos cuidados pós-natais essenciais e de rotina prestados às mulheres e aos recém-nascidos, com o objetivo final de melhorar a saúde e o bem-estar materno e neonatal.
Uma “experiência pós-natal positiva” é um resultado importante para todas as mulheres que dão à luz e para os seus recém-nascidos, estabelecendo as bases para a melhoria da saúde e do bem-estar a curto e longo prazo. Uma experiência pós-natal positiva é definida como aquela em que as mulheres, pessoas que gestam, os recém-nascidos, os casais, os pais, os cuidadores e as famílias recebem informação consistente, garantia e apoio de profissionais de saúde motivados; e onde um sistema de saúde flexível e com recursos reconheça as necessidades das mulheres e dos bebês e respeite o seu contexto cultural.
Estas diretrizes consolidadas apresentam algumas recomendações novas e já bem fundamentadas sobre cuidados pós-natais de rotina para mulheres e neonatos que recebem cuidados no pós-parto em unidades de saúde ou na comunidade, independentemente dos recursos disponíveis.
É fornecido um conjunto abrangente de recomendações para cuidados durante o período puerperal, com ênfase nos cuidados essenciais que todas as mulheres e recém-nascidos devem receber, e com a devida atenção à qualidade dos cuidados; isto é, a entrega e a experiência do cuidado recebido. Estas diretrizes atualizam e ampliam as recomendações da OMS de 2014 sobre cuidados pós-natais da mãe e do recém-nascido e complementam as atuais diretrizes da OMS sobre a gestão de complicações pós-natais.
O estabelecimento da amamentação e o manejo das principais intercorrências é contemplada.
Recomendamos muito.
Vamos discutir essas recomendações no nosso curso de pós-graduação em Aleitamento no Instituto Ciclos.
Esta publicação só está disponível em inglês até o momento.
Prof. Marcus Renato de Carvalho
www.agostodourado.com
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
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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.
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!
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.
Ozempic: Preoperative Management of Patients on GLP-1 Receptor Agonists Saeid Safari
Preoperative Management of Patients on GLP-1 Receptor Agonists like Ozempic and Semiglutide
ASA GUIDELINE
NYSORA Guideline
2 Case Reports of Gastric Ultrasound
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Ve...kevinkariuki227
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Verified Chapters 1 - 19, Complete Newest Version.pdf
TEST BANK for Operations Management, 14th Edition by William J. Stevenson, Verified Chapters 1 - 19, Complete Newest Version.pdf
2. Table of contents
Introduction
Principle of MS
Components of MS
Manipulation of MS
Components of MS
Tandem MS
Interpretation of MS
Some applications of MS in Pharmacognosy
Conclusion
References
3. Introduction
• Mass spectrometry is a physical measuring technique whose foundations were developed
in the early 20th century. Since the 1970s, and especially in the past few years, ongoing
technological developments have contributed substantially to progress in biochemistry,
molecular biology, and medicine.
• Mass spectrometry is a powerful analytical technique used to
• quantify known materials,
• to identify unknown compounds within a sample, and
• to elucidate the structure and chemical properties of different molecules.
• The complete process involves the conversion of the sample into gaseous ions, with or
without fragmentation, which are then characterized by their mass to charge ratios (m/z)
and relative abundances.
• This technique basically studies the effect of ionizing energy on molecules.
4. Basic Principles of Mass Spectrometry
MASS SPECTRUM
The formed ions are separated by deflection in Magnetic field according to their mass and
charge
Further break up onto smaller ions
(Fragment ions or Daughter ions)
Converted into Highly energetic positively charged ions
(Molecular ions or Parent ions)
Organic molecules are bombarded with electron
5. Components of Mass Spectrometry
The instrument consists of three major components:
1. Ion Source: For producing gaseous ions from the substance being studied.
2. Analyzer: For resolving the ions into their characteristics mass components according
to their mass-to-charge ratio.
3. Detector System: For detecting the ions and recording the relative abundance of each of
the resolved ionic species.
6. Manipulation of Mass Spectrometry
Manipulation in MS comprise of the following:
1. Changing the different components of mass spectrometry apparatus
•Sample Introduction (Coupling)
•Ionisation Techniques
•Mass Analysers
•Detectors
2. Tandem Mass Spectrometry (MS/MS)
8. Sample Introduction
• Direct Vapour Inlet
• Gas Chromatography
• Liquid Chromatography
• Direct Insertion Probe
• Direct Ionization of Sample
9. Sample Introduction
DVI
•Simplest Method
•Introduced by
needle
•Works for solid,
liquid & gas of
High Vapour
pressure only
GC
•Most common
technique
•Complex mixtures
can be separated
•Quantification
possible
•Pressure should be
maintained
LC
•Thermally labile
compounds
•Temperature
sensitive compds;
ionisation from
condensed phase
DIP
•Low vapour
pressure liquids &
solids sample
•Higher
temperatures
•Sample under
vacuum
•Wider range of
sample
DIoS
•Compds that
decompose &
have no sign. VP
•Introduced by
direct ionisation
from condensed
form
10. Types of ionisation techniques
• Volatile samples
• Electron Ionisation
• Chemical Ionisation
• Non-volatile samples
• Fast Atom Bombardment
• Thermospray
• Matrix Assisted Laser Desorption Ionisation
• Electrospray Ionisation
• Atmospheric Pressure Chemical Ionisation
11. Ionisation
Techniques
Volatile samples Non-Volatile samples
EI
•Heated filament emits
é; accelerated by PD of
70 eV
•Ionisation: removal of é
from molecule
•Produces +ve charged
ions with 1 unpaired é
CI
Produces M+H+ ions or
M–H- ions
Ionisation: gas
introduced; collision of
analyte with gas ions
Positive CI uses NH3
Negative CI uses CH3
FAB
•Low volatility compds
•Solid/liquids mixed
with non-Volatile
matrix: glycerol
•Bombarded with Ar or
Xe atoms
•Gives M+H+ or M+Na+
ions
TS
•Used: LC/MS
•Polar compounds
•Ionisation:LC:Sample
+ C2H3O2NH4
•Produces M+H+ or M -
H- ions
•Not commercially
available today MALDI
•Similar to FAB
•Ionisation: Sample dissolved
in matrix; absorbs light
•Coupled to TOF/MS not LC
•High mass range achievable
•Reproducibility issuesESI
•Polar non-volatile
compounds
•Coupled to LC
•Produces M+H+ or M -
H- ions
•High Mr can be
determined
APCI
• Wide range polar
cmpds
• Ionisation:
HPLC+Corona discharged
needle
• Form either M+H+ or
M-H- ions
• Thermal degradation
12. Types of Mass analysers
• There are six general types of
mass analyzers that can be used
for the separation of ions in a
mass spectrometry.
13. Quadrupole Mass Analyzer
A combination of Direct Current (DC) and
Radio Frequency (RF) voltages are applied
to two pairs of metal rods to influence ions
trajectories.
Time of Flight Mass Analyzer
Ions are accelerated by an electric field
and the times it takes for the ion to travel
over a known distance is measured.
Magnetic Sector Mass Analyzer
An ion is accelerated into a curved flight
tube where a magnet deflects the trajectory
wrt its m/e ratio
14. Electrostatic Sector Mass Analyzer
Ion travels through the electric field and the force on
the ion is equal to the centripetal force on the ion.
Here the ions of the same kinetic energy are focused,
and ions of different kinetic energies are dispersed.
Quadrupole Ion Trap Mass Analyzers
Ions are stabilised in a ring electrode containing
device (trap) by applying an Radio Frequency voltage
Ion Cyclotron Resonance
Mass-to-charge ratio (m/z) of ions are determined in a
fixed magnetic field. The ions are excited within a
Penning trap(a magnetic field with electric trapping
plates).
16. Types of detectors
Detector
s
Faraday cup
Ions strike dynode
surface; electrons
emitted=current
induced
Electron Multiplier
+ve & -ve ions
detected on same
instrument
Electron emitted
focussed
magnetically
Photomultiplier
Photons emitted
Converted to current
17. 2. Tandem Mass Spectrometry
• Tandem Mass Spectrometry, usually referred to as MS/MS, involves the use of 2 or
more mass analyzers.
• It is often used to analyze individual components in a mixture.
• This technique adds specificity to a given analysis.
• This is a powerful way of confirming the identity of certain compounds and determining
the structure of unknown species.
• So MS/MS is a process that involves 3 steps: ionization, mass selection, mass analysis.
• MS/MS could be performed on instruments such as triple quadrupole (QQQ), ion trap,
time of flight, fourier transform, etc.
• The triple quadrupole is the most frequently used mass spectrometer for MS/MS,
perhaps because of the cost and ease of use among other factors.
19. Analysis of Mass Spectra
Ester
Not
aldehyde,
ketone or
carboxylic
acid
Mr=88
M: 44
Rest of ester: 88 - 44 = 44
CH3 and C2H5
15 + 29 = 44
M:15
CH3
+
M:29
CH3CH2
+
15+44= 59
CH3COO+ or
COOCH3
+
m/z= 57 ?
M:31
O-CH3
+
M:43
CH3CO+
M:57
C2H5CO+
20. Application of MS in Pharmacognosy
• A crude plant extract may contain up to hundreds of different secondary metabolites of
considerably differing chemical nature and spectroscopic parameters.
• Therefore chromatographic, purification or isolation steps of separation are crucial prior to
detection, identification and quantification.
• Characterization and identification of unknown constituents requires a more informative,
selective and sensitive analytical tool.
• Some of the MS tools used are:
• Chromatographic techniques combined with mass spectrometry: GC-MS, LC-MS,
HPLC-MS..
• Common mass spectrometer configurations and techniques: MALDI, MALDI-TOF..
• TANDEM MS: MS/MS, GC/MS/MS, LC/MS/MS..
21. Total Phenolic by MS
• Phenolic compounds are plant secondary metabolites, which play important roles in disease
resistance
• The interest on these compounds is related with their antioxidant activity and promotion of
health benefits
• Virgin olive oil is an important dietary oil, rich in natural antioxidants
• Olives and leaves of ten olive tree cultivars (Olea europaea L.) from the region of Trás-os-
Montes e AltoDouro (Portugal) were studied: ‘Bical’, ‘Borrenta’, ‘Cobrançosa’,
‘Coimbreira’, ‘Lentisca’, ‘Madural’, ‘Negrinha de Freixo’, ‘Redondal’, ‘Santulhana’ and
‘Verdeal Transmontana’.
• HPLC Coupled with Atmospheric Pressure Chemical Ionisation (APCI) MS
• Total phenolic was determined colorimetrically at 760nm after reacting with Folin reagent;
Expressed as tannic acid.
S. Silva et al, 2006, Phenolic Compounds and Antioxidant Activity of Olea europaea L. Fruits and Leaves, Food Sci Tech
Int 2006; 12(5):385–396
22. • The type of phenolic compounds detected in leaf, fruit and seed varied
markedly.
• The high antioxidant activity of seed extracts is due to nüzhenide and related
compounds, suggesting the possible application of olive seeds as sources of
natural antioxidants.
S. Silva et al, 2006, Phenolic Compounds and Antioxidant Activity of Olea europaea L. Fruits and Leaves, Food Sci Tech
Int 2006; 12(5):385–396
Total Phenolic by MS
23. GC-MS
Four Greek endemic Boraginaceae plants, Onosma erecta Sibth. & Sm., Onosma kaheirei Teppner,
Onosma leptantha Heldr., and Cynoglossum columnae L. (aerial parts), were screened for their
content of pyrrolizidine alkaloids (PAs)- present in the form of N-Oxide; highly polar; possess
hepatotoxic, hemolytic, antimitotic, teratogenic, mutagenic, and carcinogenic effects.
• Qualitative tests by TLC
• Quantitative test by GC-MS
• Extraction of dry plant material done by using MeOH
• Liquid-liquid extraction done by CH2Cl2
• CH2Cl2 was condensed and analysed
• Results:
• 23 peaks were obtained and their structures were identified
• 100% PAs and PA-N-Oxides from C. columnae
• 100% PA-N-Oxides from O. leptantha
• No free PAs were obtained from O. erecta and O. kaheirei (Reason: Thermally decomposed)
Damianakos et al., 2014, The Chemical Profile of Pyrrolizidine Alkaloids from Selected Greek Endemic Boraginaceae
Plants Determined by Gas Chromatography/Mass Spectrometry : Journal of AOAC International Vol. 97, No. 5
24. LC-TOF/MS
• LC-TOF/MS method was developed for qualitative and quantitative
analysis of the major chemical constituents in Andrographis
paniculata. (Used for common cold, fever and non-infectious
diarrhea)
• Ultrasonic Extraction: 0.2 g plant sample extracted with 10 mL of
70% ethanol and extraction for 30 min at under 50 kHz ultrasonic
irradiation.
• LC performed; fifteen compounds, including flavonoids and
diterpenoid lactones, were unambiguously or tentatively identified in
10 min by comparing their retention times and accurate masses with
standards or literature data.
• TOF-MS done to identify the compound (eg C6: Andrographolide)
• This study would facilitate the quality evaluation of A. paniculata for
safe and efficacious use and be a powerful reference for the
identification of similar compounds presented here by MS spectra.
Yong-Xi Song, 2013, Qualitative and Quantitative Analysis of Andrographis paniculata by Rapid Resolution Liquid
Chromatography/Time-of-Flight Mass Spectrometry, Molecules 2013, 18, 12192-12207
25. HPLC-MS
• β-sitosterol is an important component in food and herbal products and beneficial in
hyperlipidemia.
• Higher conc. in serum may lead to coronary artery disease in case of sitosterolemia.
• Quantity of β-sitosterol in food and herbal drugs needs to be determined.
• Quantitative estimation of β-sitosterol present in hot and cold water extracts of bark,
regenerated bark, leaves and flowers of the S. asoca and Ashokarista drugs were carried out
first time using high performance liquid chromatography coupled (HPLC) with quadrupole
TOF-MS
• Extraction was done with deionised water for 3days; centrifuged, lyophilised and filtered.
• Different concentrations of β-sitosterol and crude extracts were estimated by HPLC and
mass spectrometry.
• The results showed significant differences in the distribution of β-sitosterol among
different organs of S. asoca.
• This type of approaches could be helpful for the quality control of herbal medicines and
provides necessary information for the rational utilization of plant resources.
Gahlaut, et al, 2013, β-sitosterol in different parts of Saraca asoca and herbal drug ashokarista: Quali-quantitative
analysis by liquid chromatography-mass spectrometry, Journal of Advanced Pharmaceutical Tech.| Jul-Sep|Vol 4:3
26. MALDI-MS
• A mass spectrometric imaging (MSI) was performed to localize
ginsenosides (Rb1, Rb2 or Rc, and Rf) in cross-sections of the Panax
ginseng root at a resolution of 100 m using matrix-assisted laser
desorption/ionization mass spectrometry (MALDI-MS).
• MALDI-MSI confirmed that ginsenosides were located more in the
cortex and the periderm than that in the medulla of a lateral root.
• In addition, it revealed that localization of ginsenosides in a root tip
(diameter, 2.7 mm) is higher than that in the center of the root
(diameter, 7.3 mm).
• A quantitative difference was detected between localizations of
protopanaxadiol-type ginsenoside (Rb1, Rb2, or Rc) and
protopanaxatriol-type ginsenoside (Rf) in the root.
• This imaging approach is a promising technique for rapid evaluation
and identification of medicinal saponins in plant tissues.
S. TAIRA et al., 2010, Mass Spectrometric Imaging of Ginsenosides Localization in Panax ginseng Root, The American
Journal of Chinese Medicine, Vol. 38, No. 3, 485–493
27. Conclusion
• Natural products (also known as secondary metabolites) have always been a
significant source of new lead compounds in pharmaceutical industries.
• Mass spectrometry has long been used in medicines.
• There are several types of MS that are use depending on the nature of the
plant extract to be analysed i.e. Volatile, polarity, temperature sensitive etc
• It is a good method for detecting, identifying and quantifying expected
metabolites using ESI, MALDI, TOF/MS, Tandem etc
• Also detect, identify and relatively quantify unexpected metabolites
• Used for Standardisation of phenolics for its antioxidants activities
(Universal protocol should be used)
• It can be used in Quality control
• Overall, MS is great tool to use in pharmacognosy: small sample size
required, fast, can be combined with GC, LC to run mixtures.
28. REFERENCES
• ‘Introduction to Mass Spectrometry’ (no date). chemwiki.ucdavis.edu. Available at:
http://chemwiki.ucdavis.edu/Analytical_Chemistry/Instrumental_Analysis/Mass_Spectrometry/Introductory_Mass_Spectrometry/I
ntroduction_to_Mass_Spectrometry (Accessed: 1 March 2015).
• Mass Spectrometry Tutorial | Chemical Instrumentation Facility (no date). Available at: http://www.cif.iastate.edu/mass-spec/ms-
tutorial (Accessed: 1 March 2015).
• S. Silva et al, 2006, Phenolic Compounds and Antioxidant Activity of Olea europaea L. Fruits and Leaves, Food Sci Tech Int 2006;
12(5):385–396
• Damianakos et al., 2014, The Chemical Profile of Pyrrolizidine Alkaloids from Selected Greek Endemic Boraginaceae Plants
Determined by Gas Chromatography/Mass Spectrometry : Journal of AOAC International Vol. 97, No. 5
• Yong-Xi Song, 2013, Qualitative and Quantitative Analysis of Andrographis paniculata by Rapid Resolution Liquid
Chromatography/Time-of-Flight Mass Spectrometry, Molecules 2013, 18, 12192-12207
• S. TAIRA et al., 2010, Mass Spectrometric Imaging of Ginsenosides Localization in Panax ginseng Root, The American Journal of
Chinese Medicine, Vol. 38, No. 3, 485–493
• Mass Spectrometry in Biotechnology by Gary Siuzdak , Academic Press 1996 SiuzdakBiotechnology”
• Mass Spectrometry in Medicine –the Role of Molecular Analyses by Michael Vogeser, Uwe Kobold, Dietrich Seidel
• An Introduction to Mass Spectrometry by Scott E. Van Bramer et al
• The Ideal Mass Analyzer: Fact or Fiction?" (Curt Brunnee, Int. J. Mass Spectrom. Ion Proc. 76 (1987), 125-237
• M. Careri et al, 2002,r ecent advances in the application of mass spectrometry in food-related analysis, Journal of Chromatography
A, 970 (2002) 3–64
Editor's Notes
Direct Vapour Inlet
The simplest sample introduction method is a direct vapour inlet.
The gas phase analyte is introduced directly into the source region of the mass spectrometer through a needle valve.
Pump out lines are usually included to remove air from the sample.
This inlet works well for gases, liquids, or solids with a high vapour pressure.
Samples with low vapour pressure are heated to increase the vapour pressure.
Since this inlet is limited to stable compounds and modest temperatures, it only works for some samples.
Gas chromatography
Gas chromatography is probably the most common technique for introducing samples into a mass spectrometer.
Complex mixtures are routinely separated by gas chromatography and mass spectrometry is used to identify and quantitate the individual components.
Several different interface designs are used to connect these two instruments.
The most significant characteristics of the inlets are the amount of GC carrier gas that enters the mass spectrometer and the amount of analyte that enters the mass spectrometer.
If a large flow of GC carrier gas enters the mass spectrometer it will increase the pressure in the source region.
Maintaining the required source pressure will require larger and more expensive vacuum pumps.
The amount of analyte that enters the mass spectrometer is important for improving the detection limits of the instrument.
Ideally all the analyte and none of the GC carrier gas would enter the source region.
Liquid chromatography
Liquid chromatography inlets are used to introduce thermally labile compounds not easily separated by gas chromatography.
These inlets have undergone considerable development and are now fairly routine.
Because these inlets are used for temperature sensitive compounds, the sample is ionized directly from the condensed phase.
Direct Insertion Probe
The Direct Insertion Probe (DIP) is widely used to introduce low vapour pressure liquids and solids into the mass spectrometer.
The sample is loaded into a short capillary tube at the end of a heated sleeve.
This sleeve is then inserted through a vacuum lock so the sample is inside the source region.
After the probe is positioned, the temperature of the capillary tube is increased to vaporize the sample.
This probe is used at higher temperatures than are possible with a direct vapour inlet.
In addition, the sample is under vacuum and located close to the source so that lower temperatures are required for analysis.
This is important for analyzing temperature sensitive compounds.
Although the direct insertion probe is more cumbersome than the direct vapour inlet, it is useful for a wider range of samples
Direct Ionization of Sample
Unfortunately, some compounds either decompose when heated or have no significant vapour pressure.
These samples may be introduced to the mass spectrometer by direct ionization from the condensed phase.
These direct ionization techniques are used for liquid chromatography/mass spectrometry, glow discharge mass spectrometry, fast atom bombardment and laser ablation.
The development of new ionization techniques is an active research area and these techniques are rapidly evolving.
Electron Ionisation
Produces M+. radical cation giving molecular weight
Produces abundant fragment ions
Library searchable spectra
Energetic process.
A heated filament emits electrons which are accelerated by a potential difference of usually 70eV into the sample chamber.
Ionisation of the sample occurs by removal of an electron from the molecule thus generating a positively charged ion with one unpaired electron.
Chemical Ionisation
Development from EI
Same compound classes as EI
Gives molecular weight
Softer ionisation technique
Produces M+H+ ions or M – H- ions
Used to produce more abundant molecular ions when the molecule under investigation fragments using EI
Similar ionisation technique to EI except that a reagent gas is introduced into the chamber in excess of the sample
Positive CI uses methane, isobutane or ammonia as reagent gases
Negative CI uses methane reagent gas in electron capture mode
Ionised reagent gas protonate the sample molecules leaving a neutral reagent gas species
Fast Atom Bombardment
Used for large compounds with low volatility (eg. peptides, proteins, carbohydrates)
Solid or liquid sample is mixed with a non-volatile matrix (eg glycerol, crown ethers, nitrobenzylalcohol)
Immobilised matrix is bombarded with a fast beam of Argon or Xenon atoms.
Charged sample ions are ejected from the matrix and extracted into the mass analysers
Gives M+H+or M+Na+ions
Choosing correct matrix is difficult
Thermospray
First widely used LC/MS interface
Flow rates 0.5 - 1.5 ml/min
Good for polar compounds
LC eluent containing sample and ammonium acetate is pumped through a heated vaporiser.
The jet of vapour contains small charged droplets which evaporate under the heat and vacuum expelling charged ions from the surface
Produces M+H+ or M - H- ions
Not commercially available today
MALDI
Similar process to FAB
Sample is dissolved in matrix which absorbs light from a short pulse of laser of a specific wavelength.
The sample becomes ionised and extracted towards the mass analysers
Coupled to Time of Flight MS
Not coupled to LC
High mass range achievable
Calibrants may be external or included in sample
Reproducibility issues
Electrospray
Electrospray also known as :Ionspray, Nanospray, Sonic Spray, “Pure” Electrospray, or ESI, E
Softest ionisation technique
Best for polar non-volatile compounds (proteins, peptides, nucleic acids, Pharmaceuticals, natural products)
Coupled to LC at a flow range of 2-1000 ul/min, nanospray (10 nL/min – 2 uL/min)
Ions are ejected from charged vapour droplets to gas phase producing M+H+ or M - H- ions
Can produce multiply charged ions allowing determination of high molecular weight proteins
Not very tolerant of non-volatile salts
APCI
Atmospheric Pressure Chemical Ionisation, also known
as : APCI, Heated nebuliser or APcl
Used for wide range polarity of compounds
HPLC eluent (up to 2ml/min flow rate) is vaporised at up to 600oC
The Corona discharge needle ionises solvent molecules.
A combination of collisions and charge transfer reactions between the solvent and the analyte results in the transfer of a proton to form either M+H+ or M-H- ions
Compounds can thermally degrade
Multiply charged ions rare
More tolerant to salt
Faraday cup
The basic principle is that the incident ion strikes the dynode surface which emits electrons and induces a current which is amplified and recorded. The dynode electrode is made of a secondary emitting material like CsSb, GaP or BeO. It is ideally suited to isotope analysis
Electron Multiplier
Electron multipliers are the most common especially when positive and negative ions need to be detected on the same instrument. Dynodes made up of copper-beryllium which transduces the initial ion current ,and electron emitted by first dynode are focused magnetically from dynode to the next. Final cascade current is amplified more than million times.
Photomultiplier
The dynode consists of a substance( a scintillator) which emits photons(light). The emitted light is detected by photo multiplier tube and is converted into electric current. These detectors are useful in studies on metastable ions
Faraday cup
The basic principle is that the incident ion strikes the dynode surface which emits electrons and induces a current which is amplified and recorded. The dynode electrode is made of a secondary emitting material like CsSb, GaP or BeO. It is ideally suited to isotope analysis
Electron Multiplier
Electron multipliers are the most common especially when positive and negative ions need to be detected on the same instrument. Dynodes made up of copper-beryllium which transduces the initial ion current ,and electron emitted by first dynode are focused magnetically from dynode to the next. Final cascade current is amplified more than million times.
Photomultiplier
The dynode consists of a substance( a scintillator) which emits photons(light). The emitted light is detected by photo multiplier tube and is converted into electric current. These detectors are useful in studies on metastable ions
The sample is acetone. On the horizontal axis is the value for m/z (as we stated above, the charge z is almost always +1, so in practice this is the same as mass). On the vertical axis is the relative abundance of each ion detected. On this scale, the most abundant ion, called the base peak, is set to 100%, and all other peaks are recorded relative to this value. For acetone, the base peak is at m/z = 43 - we will discuss the formation of this fragment a bit later. The molecular weight of acetone is 58, so we can identify the peak at m/z = 58 as that corresponding to the molecular ion peak, or parent peak. Notice that there is a small peak at m/z = 59: this is referred to as the M+1 peak. How can there be an ion that has a greater mass than the molecular ion? Simple: a small fraction - about 1.1% - of all carbon atoms in nature are actually the 13C rather than the 12C isotope. The 13C isotope is, of course, heavier than 12C by 1 mass unit. In addition, about 0.015% of all hydrogen atoms are actually deuterium, the 2H isotope. So the M+1 peak represents those few acetone molecules in the sample which contained either a 13C or 2H.
Saponins are glucosides with foaming characteristics. Saponins consist of a polycyclic aglycones attached to one or more sugar side chains. The aglycone part, which is also called sapogenin, is either steroid (C27) or a triterpene (C30). The foaming ability of saponins is caused by the combination of a hydrophobic (fat-soluble) sapogenin and a hydrophilic (water-soluble) sugar part. Saponins have a bitter taste. Some saponins are toxic and are known as sapotoxin.
Health benefits: Antioxidants, anti cancer, cholesterol reducing
Panax ginseng used for stress, memory, depression, anxiety, breast cancer