LC-MS is a technique that combines liquid chromatography and mass spectrometry. It separates components in a mixture using HPLC and then uses an ion source like ESI or APCI to ionize the molecules and a mass analyzer like a quadrupole or time-of-flight to separate the ions by mass-to-charge ratio. The ions are then detected to identify and quantify each component. Validation of the LC-MS system involves tests of the vacuum, mass accuracy, linearity, precision, carryover, and signal-to-noise ratio to ensure proper operation and performance.
Using LC-MS/MS and Advanced Software Tools to Screen for unknown and Non-targ...AB SCIEX India
LC-MS/MS is a powerful tool for the analysis of Pharmaceuticals and Personal Care Products in environmental samples. The combination of high resolution LC separation and high sensitivity MS/MS is the most powerful tool to screen and quantify targeted compounds.
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.
Detectors are the brain of any chromatograhic system. It help us to record the chromatogram based on certain characteristics of the analyte and help us in identifying that compound both qualitatively and quantitatively.
Using LC-MS/MS and Advanced Software Tools to Screen for unknown and Non-targ...AB SCIEX India
LC-MS/MS is a powerful tool for the analysis of Pharmaceuticals and Personal Care Products in environmental samples. The combination of high resolution LC separation and high sensitivity MS/MS is the most powerful tool to screen and quantify targeted compounds.
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.
Detectors are the brain of any chromatograhic system. It help us to record the chromatogram based on certain characteristics of the analyte and help us in identifying that compound both qualitatively and quantitatively.
HPLC is Analytical technique that is used for separating the mixture of substances,so there is a number of promising application of HPLC-UV here uv detector is used which record the absorbance
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 versatile instrument is used to isolate unknown compounds from a HPTLC/TLC plate and transfer them into a mass spectrometer for identification or structure elucidation.
• 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.
an overview of lcms and gcms and its applications....
LC-MS:
It is the combination of liquid chromatography and the mass spectrometry.
* In LC-MS we are removing the detector from the column of LC and fitting the column to interface of MS.
* In the most of the cases the interface used in LC-MS are ionization source
INTERFACE
Apart from being an inlet system for the
MS, an LC–MS interface is also the coupling
of a detector (MS) to a chromatograph.
The choice of LC–MS interface strongly
influences the characteristics of the MS as
a detector for LC. Therefore, we should
keep in mind what characteristics are ideal
for an LC detector
1. Direct liquid introduction (DLI):
The DLI interface was developed in order to solve the problems with in-capillary evaporation in the capillary inlet.
In a DLI interface, the column effluent is nebulized by the disintegration into small droplets of a liquid jet formed at a small diaphragm After desolvation of the droplets in a desolvation chamber, the analytes can be analysed using solvent-mediated CI with the LC solvents as the reagent gas.
Advantages:
• No heat is applied to the interface and it is therefore able to deal with thermally labile materials better than the moving-belt interface.
• The interface contains no moving parts and is cheap and simple to construct and operate and is inherently more reliable than the moving-belt interface.
• Both positive- and negative-ion CI spectra can be generated and the interface provides molecular weight information, plus it can also be used for sensitive quantitative and semi-quantitative procedures.
Disadvantages:
• Involatile compounds are not usually ionized with good efficiency.
• The pinhole is prone to blockage and therefore the system must be kept completely free of solid materials.
• Only a small proportion of the flow from a conventional HPLC column is able to enter the source of the mass spectrometer and sensitivity is consequently low
2. Moving belt/wire:
In a moving-belt interface (MBI), the column effluent is deposited onto an endless moving belt from which the solvent is evaporated by means of gentle heating and efficiently exhausting the solvent vapours. After removal of the solvents, the analyte molecules are (thermally) desorbed from the belt into the ion source and mass analysed.
The MBI for LC.MS was used in a wide variety of applications, including the analysis of drugs and their metabolites, pesticides, steroids, alkaloids, polycyclic, aromatic hydrocarbons and others.
Advantages:
• The interface can be used with a wide range of HPLC conditions.
• The analyst does have some choice of the ionization method to be used; EI, CI and FAB are available, subject to certain limitations, and thus both molecular weight and structural information may be obtained from the analyte(s) under investigation.
mass spectrometry for pesticides residue analysis- L1sherif Taha
This is the first lecture in series of lectures on mass spectrometry for pesticides residue analysis. This lecture (1) include Pesticides classification, introduction to mass spectrometry, vacuum system for Agilent GC MS/ MS and AB SCIEX LC MS/ MS
1. It is one of the type of Hyphenated technique.
2. It is a combination of gas chromatographic technique and spectroscopic technique.
3. It is having a high resolution capacity.
4. It is used has volatile and Non-volatile compounds.
5. It is used for qualitative and quantitative analysis.
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.
HPLC is Analytical technique that is used for separating the mixture of substances,so there is a number of promising application of HPLC-UV here uv detector is used which record the absorbance
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 versatile instrument is used to isolate unknown compounds from a HPTLC/TLC plate and transfer them into a mass spectrometer for identification or structure elucidation.
• 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.
an overview of lcms and gcms and its applications....
LC-MS:
It is the combination of liquid chromatography and the mass spectrometry.
* In LC-MS we are removing the detector from the column of LC and fitting the column to interface of MS.
* In the most of the cases the interface used in LC-MS are ionization source
INTERFACE
Apart from being an inlet system for the
MS, an LC–MS interface is also the coupling
of a detector (MS) to a chromatograph.
The choice of LC–MS interface strongly
influences the characteristics of the MS as
a detector for LC. Therefore, we should
keep in mind what characteristics are ideal
for an LC detector
1. Direct liquid introduction (DLI):
The DLI interface was developed in order to solve the problems with in-capillary evaporation in the capillary inlet.
In a DLI interface, the column effluent is nebulized by the disintegration into small droplets of a liquid jet formed at a small diaphragm After desolvation of the droplets in a desolvation chamber, the analytes can be analysed using solvent-mediated CI with the LC solvents as the reagent gas.
Advantages:
• No heat is applied to the interface and it is therefore able to deal with thermally labile materials better than the moving-belt interface.
• The interface contains no moving parts and is cheap and simple to construct and operate and is inherently more reliable than the moving-belt interface.
• Both positive- and negative-ion CI spectra can be generated and the interface provides molecular weight information, plus it can also be used for sensitive quantitative and semi-quantitative procedures.
Disadvantages:
• Involatile compounds are not usually ionized with good efficiency.
• The pinhole is prone to blockage and therefore the system must be kept completely free of solid materials.
• Only a small proportion of the flow from a conventional HPLC column is able to enter the source of the mass spectrometer and sensitivity is consequently low
2. Moving belt/wire:
In a moving-belt interface (MBI), the column effluent is deposited onto an endless moving belt from which the solvent is evaporated by means of gentle heating and efficiently exhausting the solvent vapours. After removal of the solvents, the analyte molecules are (thermally) desorbed from the belt into the ion source and mass analysed.
The MBI for LC.MS was used in a wide variety of applications, including the analysis of drugs and their metabolites, pesticides, steroids, alkaloids, polycyclic, aromatic hydrocarbons and others.
Advantages:
• The interface can be used with a wide range of HPLC conditions.
• The analyst does have some choice of the ionization method to be used; EI, CI and FAB are available, subject to certain limitations, and thus both molecular weight and structural information may be obtained from the analyte(s) under investigation.
mass spectrometry for pesticides residue analysis- L1sherif Taha
This is the first lecture in series of lectures on mass spectrometry for pesticides residue analysis. This lecture (1) include Pesticides classification, introduction to mass spectrometry, vacuum system for Agilent GC MS/ MS and AB SCIEX LC MS/ MS
1. It is one of the type of Hyphenated technique.
2. It is a combination of gas chromatographic technique and spectroscopic technique.
3. It is having a high resolution capacity.
4. It is used has volatile and Non-volatile compounds.
5. It is used for qualitative and quantitative analysis.
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.
Part of of a series of technical seminars held at my institute. My presentation focused on the use of mass spectrometry in the analysis of biological samples.
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
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.
No single liquid chromatography (LC) detector delivers ideal results. Often with LC detectors one analyte responds more strongly than another, or may not respond at all. What is most desired is the ability to accurately measure a wide range of analytes with consistent response simultaneously.
Charged Aerosol detection (CAD) is a mass sensitive technique for determining levels of any non-volatile and many semi-volatile analytes after separation by liquid chromatography. This technique provides consistent analyte response independent of chemical characteristics and gives greater sensitivity over a wider dynamic range. An analytes response does not depend on optical properties, like with UV-vis absorbance, or the ability to ionize, as with mass spectrometry (MS). The presence of chromophoric groups, radiolabels, ionizable moieties, or chemical derivatization is needed for detection.
Presentation Outline for Expanding Your High Performance Liquid Chromatography and Ultra High Performance Liquid Chromatography Capabilities with Universal Detection-Shedding Light on Non-Chromophore Compounds:
• Introduction to Charged Aerosol Detection
• How Charged Aerosol Technology Works
• Comparison with Evaporative Light Scattering Detectors
(ELSD)
• Examples of Applications
• Inverse Gradient Solution for Uniform Response
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.
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.
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.
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.
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.
This pdf is about the Schizophrenia.
For more details visit on YouTube; @SELF-EXPLANATORY;
https://www.youtube.com/channel/UCAiarMZDNhe1A3Rnpr_WkzA/videos
Thanks...!
2. LIQUID CHROMATOGRAPHY
MASS SPECTROMETRY
•Liquid chromatography-mass spectrometry (LC/MS) is a
technique that uses liquid chromatography (or HPLC) with
the mass spectrometry.
•It is an analytical chemistry technique that combines the
physical separation capabilities of liquid chromatography
with the mass analysis capabilities of mass spectrometry.
3. PRINCIPLE
•The LC-MS technology involves use of an HPLC, wherein
individual components in a mixture are first separated
followed by ionization and separation of the ions on the
basis of their mass/charge ratio. The separated ions are
then directed to a photo multiplier tube detector, which
identifies and quantifies each ion. The ion source is an
important component in any MS analysis, as this basically
aids in efficient generation of ions for analysis. To ionize
intact molecules, the ion source could be APCI
(Atmospheric Pressure Chemical Ionization), ESI
(Electronspray Ionization), etc. to name a few popular
ones. The choice of ion source also depends on the
chemical nature of the analyte of interest i.e. polar or non-
polar.
5. 1. Ion source, which can convert gas phase sample
molecules into ions.
Following are the most common ionization methods
:
i. Electrospray Ionization
ii. Atmospheric Pressure Chemical Ionization
iii. Atmospheric Pressure Photo-ionisation
Components of Mass Spectrometer :
6. Components of Mass Spectrometer :
2. Analyzer , where ions are separated according to their
mass-to-charge ratio by applying electromagnetic fields.
•Its task is to separate ions in terms of their mass-to charge
•ratio and to direct the beam of focused ions to the detector.
•The key performance parameters of an analyzer include;
(a) separation efficiency
(b) m/z measurement precision
(c) range of the m/z values measured
•There are following kinds of mass analyzers that can be used
in LC/MS : (a)
Quadrupole Analyzer, (b)
Time-of-Flight Analyzer, (c) Ion
Trap Analyzer
7. Components of Mass Spectrometer :
3. Detectors :
The detector is used to count the ions emergent from
the mass analyzer, and may also amplify the signal
generated from each ion. Following are three different
kinds of detectors are used in Mass Spectrometry;
(a)Electron Multipliers (b)Dynolyte
Photomultiplier:
8. Tandem Mass Spectrometry
• Tandem mass spectrometry (MS/MS) is a system of two combined
analyzers of the same type or different types, characterized by high
separation efficiency.
• The ions produced by the source are separated in the first analyzer
(MS1). Ions with the selected m/z value reach the collision cell
where, depending on the analysis conditions, they undergo
dissociation or remain unchanged.
• In comparison with analysis using a single analyzer, tandem analysis
shows a considerable improvement in selectivity and considerably
increased sensitivity
9. OQ—Operational
Qualification
• Temperature accuracy and stability of column heater/cooler
• Holmium oxide wavelength scan (if applicable)
• Detector lamp intensity and wavelength accuracy
• Detector noise and drift
• Pump flow rate accuracy and repeatability
• High and low pressure shutdown accuracy
• Injector precision
• Detector linearity and sampleto-sample carryover
• Injection volume linearity
• Gradient composition accuracy
• Linear gradient tested using IPA and 0.5% Acetone/IPA
• Five step gradient tested using IPA and 0.5% Acetone/IPA
11. PQ—Performance
Qualification
• System performance and robustness
• Typically a 5 or 10 μL injection of a low
concentration sample, repeated five times
• Compare area count and retention time
deviations
12. Tests for HPLC Systems (Non-MSD)
Test Name Setpoints and
Parameters
Limits
Vacuum
Verification
N/A High vacuum min.: 8E-6 torr (any source)
High vacuum max.: 4E-5 torr (any source),
Scan
Verification
All used masses: ± 3.0 ppm (DSES, ES+AJST;
N/A for others)
Response
Linearity
Evaluated mass: 156
m/z Injection volume
on column: 20 ul*
Coefficient of determination (r2): ≥ 0.98000
(DSES, ES+AJST; N/A for others)
13. Tests for HPLC Systems (Non-MSD)
Test Name Setpoints and Parameters Limits
Injection
Precision
Evaluated mass: 156 m/z
Injection volume on
column: 20 ul*
Area RSD: ≤ 20.00 % (any source)
Height RSD: Not applicable (any
source)
Injection Carry
Over
Evaluated mass: 156 m/z
Injection volume on
column: 20 ul*
Area & height carry over ≤ 1.00 %
(DSES, ES+AJST;
N/A for others)
Signal to Noise
Evaluated mass: 156 m/z
Injection volume on
column: 20 ul*
Signal to noise: ≥ 10 (DSES,
ES+AJST; N/A for others)
14. Tests for Mass Spectrometer Detectors of
LCMS:
MSD 1. Vacuum Verification
Rationale: A stable, high vacuum is required for high-sensitivity mass
spectrometry.
Procedure: Multiple readings of the vacuum system are taken and an
automated comparison of these values to the known acceptable values is
made. Passing this test is a pre-requisite for the following tests.
MSD 2. Scan Verification
Rationale: Calibration of mass range is critical in qualitative mass
spectrometry.
Procedure: [Agilent LCMS] The built-in Agilent autotune is performed to
determine the proper calibration of the MSD and ensure that masses are
correctly reported across the entire mass range of the instrument. [Non-
Agilent LCMS] A manual tune is made where applicable.
15. Tests for Mass Spectrometer
Detectors of LCMS:
MSD 3. Response Linearity
Rationale: Knowledge of the response curve is critical for quantitative analysis.
Procedure: A sulfa drug mix standard of four sulfonamide drugs is injected into
the system at five concentrations representing a wide range for LCMS. The ions
monitored are appropriate to the system type. The calculated RSQ best-fit
regression line and plot of the response curve provides the statistics required to
evaluate the instrument’s overall response curve. This allows users to set
appropriate calibration ranges and limits in their quantitative application
methods.
MSD 4. Injection Precision
Rationale: System precision is critical for accuracy of quantitation. Autosampler
performance and MS ionization contribute to LCMS system precision.
Autosampler precision is challenged in the standard LC module tests using a UV
detector. A repeat precision test in MS mode further challenges the precision of
source ionization and MS detection. Procedure: A blank injection followed by six
repeat injections of the sulfa drug mix followed by a final blank injection are
made. The %RSD of the six injections is calculated to provide precision statistics.
16. Tests for Mass Spectrometer
Detectors of LCMS:
MSD 5. Carry Over
Rationale: Low carry over from a previous injection is critical for accuracy of
quantitative and reliability of qualitative analysis. Autosampler performance and
MSD condition contribute to LCMS carry over. Autosampler carry over is
challenged in the standard LC module tests using a UV detector. A repeat carry
over test in MS mode further challenges the full LCMS system carry over
performance.
Procedure: A blank injection followed by single injection of the highest
concentration standard followed by a blank injection. The last blank injection is
evaluated for carry over and the result expressed as a percentage of the value for
the standard injection.
MSD 6. Signal to Noise
Rationale: Sensitivity of MS detection is an important performance feature in
quantitative and qualitative analysis. A signal-to-noise value of representative
compounds and appropriate ions at known concentration provides sensitivity
statistics