This document discusses strategies for designing an extractables and leachables study for a packaging system. It provides background on identifying materials of construction, extraction conditions to mimic use conditions, qualitative analytical techniques, and identification of unknown extracts. The strategies include cut-and-cover extraction, full fill extraction, one-sided extraction, and large volume dynamic headspace analysis. Identification involves database searches, molecular formula generation, and MS/MS or CI fragmentation.
Practical Implementation of the New Elemental Impurities Guidelines May 2015SGS
The International Conference on Harmonization (ICH) released its Q3D Guideline for Elemental Impurities in December 2014, initiating reviews and changes in quality testing programs in bio/pharmaceutical companies around the world. In advance of the implementation dates, companies need to assess the risks of potential elemental impurities in their process and materials streams.
In this presentation, experts will review the requirements of elemental impurities guidelines from ICH, the European Pharmacopeia, and United States Pharmacopeia, outline practical recommendations to address implementation challenges, and discuss key considerations for analytical testing programs.
Particles in the Biotech Product Life Cycle: Analysis, Identification and Con...SGS
This presentation looks at the different technologies available for detection of particles generated during the drug development lifecycle and their control using a formulation approach for particles generated as a result of agitation and freeze/thaw, events commonly observed during sample shipment and temperature excursions.
Q3D - Elemental Impurities: What implications for APIs & excipients suppliers?Quality Assistance s.a.
ICH Q3D Step4 will have to be applied very soon: June 2016 for new Drug Products and
1st January 2018 for all existing DP, making it mandatory for all manufacturers to carry out a risk assessment to control elemental impurities in their DP.
Such evaluation needs to consider all potential sources of Elemental Impurities and obviously, drug product components are probably the most likely contributors.
by Dr Ph. De Raeve, Scientific Director
For more informations : www.quality-assistance.com
Practical Implementation of the New Elemental Impurities Guidelines May 2015SGS
The International Conference on Harmonization (ICH) released its Q3D Guideline for Elemental Impurities in December 2014, initiating reviews and changes in quality testing programs in bio/pharmaceutical companies around the world. In advance of the implementation dates, companies need to assess the risks of potential elemental impurities in their process and materials streams.
In this presentation, experts will review the requirements of elemental impurities guidelines from ICH, the European Pharmacopeia, and United States Pharmacopeia, outline practical recommendations to address implementation challenges, and discuss key considerations for analytical testing programs.
Particles in the Biotech Product Life Cycle: Analysis, Identification and Con...SGS
This presentation looks at the different technologies available for detection of particles generated during the drug development lifecycle and their control using a formulation approach for particles generated as a result of agitation and freeze/thaw, events commonly observed during sample shipment and temperature excursions.
Q3D - Elemental Impurities: What implications for APIs & excipients suppliers?Quality Assistance s.a.
ICH Q3D Step4 will have to be applied very soon: June 2016 for new Drug Products and
1st January 2018 for all existing DP, making it mandatory for all manufacturers to carry out a risk assessment to control elemental impurities in their DP.
Such evaluation needs to consider all potential sources of Elemental Impurities and obviously, drug product components are probably the most likely contributors.
by Dr Ph. De Raeve, Scientific Director
For more informations : www.quality-assistance.com
Stability indicating method development and validation for the simultaneous e...pharmaindexing
Stability indicating method development and validation for the simultaneous estimation of rabeprazole sodium and ketorolac tromethamine in bulk and synthetic mixture by RP-HPLC
Quality-by-design-based development and validation of a stability-indicating ...Ratnakaram Venkata Nadh
A systematic design-of-experiments was performed by applying quality-by-design concepts to determine
design space for rapid quantification of teriflunomide by the ultraperformance liquid chromatography
(UPLC) method in the presence of degradation products. Response surface and central composite
quadratic were used for statistical evaluation of experimental data using a Design-Expert software. The
response variables such as resolution, retention time, and peak tailing were analyzed statistically for the
screening of suitable chromatographic conditions. During this process, various plots such as perturbation,
contour, 3D, and design space were studied. The method was developed through UPLC BEH C18
2.1 � 100 mm, 1.7-μ column, mobile phase comprised of buffer (5 mM K2HPO4 containing 0.1%
triethylamine, pH 6.8), and acetonitrile (40:60 v/v), the flow rate of 0.5 mL min 1 and UV detection at
250 nm. The method was developed with a short run time of 1 min. Forced degradation studies revealed
that the method was stability-indicating, suitable for both assay and in-vitro dissolution of a drug product.
The method was found to be linear in the range of 28–84 μg mL 1, 2.8–22.7 μg mL 1 with a correlation
coefficient of 0.9999 and 1.000 for assay and dissolution, respectively. The recovery values were found in
the range of 100.1–101.7%. The method was validated according to ICH guidelines.
This presentation compares two United States Pharmacopial Convention (USP) regulations, 735 and 233, and their usefulness for performing elemental impurity analysis in pharmaceutical products. Conclusions are drawn based on performance, price and efficiency. For more info, go to www.ssi.shimadzu.com. Thanks for viewing.
Considerations to Extractables and Leachables Testing SGS
How to organize Extractables Assessments? FDA continues to issue Warning Letters to companies that fail to properly complete Design Verification, Design Validation, and Process Validation, and recently to include failures of manufacturers in Risk Management. The evaluation of extractables and leachables has become an increasingly important aspect in the Quality by Design (QbD) initiative of the FDA in the area of drug product design, including materials used in the drug product production process and container and closure systems used for product packaging. This presentation provides general approaches and practical aspects in E&L testing.
Pesticide residue detection methods by making use of the quantum related technologies are described, the motivation is to push the detection limit, to protect the environment we are to survive beyond what Stephen Hawking predicted!
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Formulation and evaluation of FDT and HPLC method development of Amlodipine b...pooja deshmukh
formulation and evaluation of fast disintegrating tablet by using superdisintegrants and RP-HPLC method development of prepered tablet of Amlodipine besilate and Candesartan cilexetil
Stability indicating method development and validation for the simultaneous e...pharmaindexing
Stability indicating method development and validation for the simultaneous estimation of rabeprazole sodium and ketorolac tromethamine in bulk and synthetic mixture by RP-HPLC
Quality-by-design-based development and validation of a stability-indicating ...Ratnakaram Venkata Nadh
A systematic design-of-experiments was performed by applying quality-by-design concepts to determine
design space for rapid quantification of teriflunomide by the ultraperformance liquid chromatography
(UPLC) method in the presence of degradation products. Response surface and central composite
quadratic were used for statistical evaluation of experimental data using a Design-Expert software. The
response variables such as resolution, retention time, and peak tailing were analyzed statistically for the
screening of suitable chromatographic conditions. During this process, various plots such as perturbation,
contour, 3D, and design space were studied. The method was developed through UPLC BEH C18
2.1 � 100 mm, 1.7-μ column, mobile phase comprised of buffer (5 mM K2HPO4 containing 0.1%
triethylamine, pH 6.8), and acetonitrile (40:60 v/v), the flow rate of 0.5 mL min 1 and UV detection at
250 nm. The method was developed with a short run time of 1 min. Forced degradation studies revealed
that the method was stability-indicating, suitable for both assay and in-vitro dissolution of a drug product.
The method was found to be linear in the range of 28–84 μg mL 1, 2.8–22.7 μg mL 1 with a correlation
coefficient of 0.9999 and 1.000 for assay and dissolution, respectively. The recovery values were found in
the range of 100.1–101.7%. The method was validated according to ICH guidelines.
This presentation compares two United States Pharmacopial Convention (USP) regulations, 735 and 233, and their usefulness for performing elemental impurity analysis in pharmaceutical products. Conclusions are drawn based on performance, price and efficiency. For more info, go to www.ssi.shimadzu.com. Thanks for viewing.
Considerations to Extractables and Leachables Testing SGS
How to organize Extractables Assessments? FDA continues to issue Warning Letters to companies that fail to properly complete Design Verification, Design Validation, and Process Validation, and recently to include failures of manufacturers in Risk Management. The evaluation of extractables and leachables has become an increasingly important aspect in the Quality by Design (QbD) initiative of the FDA in the area of drug product design, including materials used in the drug product production process and container and closure systems used for product packaging. This presentation provides general approaches and practical aspects in E&L testing.
Pesticide residue detection methods by making use of the quantum related technologies are described, the motivation is to push the detection limit, to protect the environment we are to survive beyond what Stephen Hawking predicted!
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Formulation and evaluation of FDT and HPLC method development of Amlodipine b...pooja deshmukh
formulation and evaluation of fast disintegrating tablet by using superdisintegrants and RP-HPLC method development of prepered tablet of Amlodipine besilate and Candesartan cilexetil
Common Mistakes in the Medical Device Development ContinuumNAMSA
Getting a medical device to market is a long process made up of multiple stages. Each stage requires a number of elements that need to be considered before progress can be made with the device. And even after market approval has been obtained, there is a continuous need to reevaluate and test the device to maintain safety and efficacy.
Throughout this development process, several steps can be missed that may result in submission refusal, or possibly a faulty device.
Understanding How Bioburden and Sterilization Affect Medical DevicesPacific BioLabs
This presentation covers:
Bioburden- what is it and how it can affect a device development program and sterilization validation program.
Sterilization: methods and the bioburden-sterilization connection.
Benefits of minimizing the sterilization dose for your device.
Importance of monitoring bioburden.
Case study: sterilization failure and tracking down root cause.
How to monitor and reduce bioburden levels.
New guidelines relating to elemental impurities from the International Conference on Harmonization (ICH), Q3D Guideline for Elemental Impurities have presented the pharmaceutical industry with new challenges. This new guidance has been developed to provide a global policy for limiting metal impurities qualitatively and quantitatively in drug products and ingredients.
20160219 - M. Agostini - Nuove tecnologie per lo studio del DNA tumorale libe...Roberto Scarafia
Nano Inspired Biomedicine Laboratory
1 Department of Surgical, Oncological and Gastroenterological Sciences, University of Padua, Italy.
2 Istituto di Ricerca Pediatrica- Città della Speranza, Padova, Italy.
Method development for the analysis of mono-carbonyl compounds in e-vapor pro...Rana Tayyarah
A robust method for ecigarette FDA-CTP PMTA guidance analytes:
formaldehyde, acetaldehyde, acrolein, crotonaldehyde
This presentation also includes details related to method optimization experiments.
2020_ST03_ZhuJ copy.pdf
Determination of Common Counterions and Impurity Anions in Pharmaceuticals Using a Capillary HPIC System with Suppressed Conductivity and Charge Detection
Recently, identification and quantification of ions in early stage drug development has gained increasing attention, because the APIs maybe contaminated with different counter ions from synthesis steps, and because selecting the counter ion to enhance APIs’ solubility and stability is becoming a key step in formulation development. This presentation demonstrates the identification and quantification of 22 commonly found anions in pharmaceuticals in a single run using a high-pressure capillary IC system (HPIC) with 4-μm particle ion –exchange column, and CD-QD dual detectors.
The ACQUITY Advanced Polymer Chromatography (APC™) System is a breakthrough technology that defines the ultimate in size-based chromatographic separations, delivering more information about your polymers faster than ever before. This means better characterization, improved asset utilization and a superior solution for achieving corporate innovation and sustainability goals.
Implementing a Fully Single-Use, Integrated mAb Biosimilars Purification Plat...MilliporeSigma
Access the interactive recording here: https://bit.ly/2DONZaQ
Webinar summary:
1000L-scale implementation of fully connected, disposable, advanced DSP platform for next generation mAb production.
Within the biopharmaceutical industry, there is a significant shift toward higher productivity processes resulting in improved economics without compromising robustness. Therefore, integrated continuous production technologies are of greatest interest.
Next Generation Biopharmaceutical Downstream Process is a European-funded collaborative project that aims at implementing a fully integrated manufacturing platform for biosimilar mAb based on continuous chromatography, in combination with single-use disposable technologies for all unit operations of DSP on pilot/small production scale together with incorporation of advanced analytical tools.
In this webinar, you will see:
* new DSP purification template producing > 3.3 kg of mAb in 2.5 days in less than 30m²
* proof of concept for the mAb manufacturing of tomorrow
Implementing a Fully Single-Use, Integrated mAb Biosimilars Purification Plat...Merck Life Sciences
Access the interactive recording here: https://bit.ly/2DONZaQ
Webinar summary:
1000L-scale implementation of fully connected, disposable, advanced DSP platform for next generation mAb production.
Within the biopharmaceutical industry, there is a significant shift toward higher productivity processes resulting in improved economics without compromising robustness. Therefore, integrated continuous production technologies are of greatest interest.
Next Generation Biopharmaceutical Downstream Process is a European-funded collaborative project that aims at implementing a fully integrated manufacturing platform for biosimilar mAb based on continuous chromatography, in combination with single-use disposable technologies for all unit operations of DSP on pilot/small production scale together with incorporation of advanced analytical tools.
In this webinar, you will see:
* new DSP purification template producing > 3.3 kg of mAb in 2.5 days in less than 30m²
* proof of concept for the mAb manufacturing of tomorrow
Over the past decade, the number of mAb candidates entering the clinical pipeline has grown significantly. In addition, the number of ADCs that use mAb specificity to carry drug payloads to target sites has increased. As a result, analytical characterization is in high demand.
This webinar discusses new innovations in sample preparation, column technology, UHPLC, and high resolution mass spectroscopy (HRMS) that allow the development of analytical methods with run times of less than 5 minutes for all routine methods.
Key Learning Objectives:
• Identify emerging triple quadrupole Gas Chromatography-Mass Spectrometry/Mass Spectrometry (GC-MS/MS) technology designed to address increasing regulatory demands and requirements
• Explore potential time savings in sample prep, method development/transition, and data analysis
• Demonstrate how to optimize the GC-MS/MS workflow from sample prep to sample analysis to automated data analysis
Overview:
Regulatory lab requirements continue to drive detection limits lower with an ever increasing list of compounds to analyze. These requirements also demand greater precision at these lower limits. Triple quadrupole GC-MS/MS is a viable option for enhanced analysis and increased productivity with an emphasis on simplicity. We discuss emerging trends and technologies designed to ensure that laboratories are well-equipped to address these increased demands with minimal investment in training and method development. Find out how you can adopt triple quadrupole GC-MS/MS technology in your laboratory using existing methods and source parameters in most instances while requiring less sample prep and enjoying the benefits of automated data analysis for increased simplicity and productivity.
For more information: www.thermoscientific.com/tsq8000
Similar to Jordi Labs Agilent Extractables & Leachables Webinar Presentation (Part 1) (20)
Professional air quality monitoring systems provide immediate, on-site data for analysis, compliance, and decision-making.
Monitor common gases, weather parameters, particulates.
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.
DERIVATION OF MODIFIED BERNOULLI EQUATION WITH VISCOUS EFFECTS AND TERMINAL V...Wasswaderrick3
In this book, we use conservation of energy techniques on a fluid element to derive the Modified Bernoulli equation of flow with viscous or friction effects. We derive the general equation of flow/ velocity and then from this we derive the Pouiselle flow equation, the transition flow equation and the turbulent flow equation. In the situations where there are no viscous effects , the equation reduces to the Bernoulli equation. From experimental results, we are able to include other terms in the Bernoulli equation. We also look at cases where pressure gradients exist. We use the Modified Bernoulli equation to derive equations of flow rate for pipes of different cross sectional areas connected together. We also extend our techniques of energy conservation to a sphere falling in a viscous medium under the effect of gravity. We demonstrate Stokes equation of terminal velocity and turbulent flow equation. We look at a way of calculating the time taken for a body to fall in a viscous medium. We also look at the general equation of terminal velocity.
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.
Salas, V. (2024) "John of St. Thomas (Poinsot) on the Science of Sacred Theol...Studia Poinsotiana
I Introduction
II Subalternation and Theology
III Theology and Dogmatic Declarations
IV The Mixed Principles of Theology
V Virtual Revelation: The Unity of Theology
VI Theology as a Natural Science
VII Theology’s Certitude
VIII Conclusion
Notes
Bibliography
All the contents are fully attributable to the author, Doctor Victor Salas. Should you wish to get this text republished, get in touch with the author or the editorial committee of the Studia Poinsotiana. Insofar as possible, we will be happy to broker your contact.
What is greenhouse gasses and how many gasses are there to affect the Earth.moosaasad1975
What are greenhouse gasses how they affect the earth and its environment what is the future of the environment and earth how the weather and the climate effects.
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.
THE IMPORTANCE OF MARTIAN ATMOSPHERE SAMPLE RETURN.Sérgio Sacani
The return of a sample of near-surface atmosphere from Mars would facilitate answers to several first-order science questions surrounding the formation and evolution of the planet. One of the important aspects of terrestrial planet formation in general is the role that primary atmospheres played in influencing the chemistry and structure of the planets and their antecedents. Studies of the martian atmosphere can be used to investigate the role of a primary atmosphere in its history. Atmosphere samples would also inform our understanding of the near-surface chemistry of the planet, and ultimately the prospects for life. High-precision isotopic analyses of constituent gases are needed to address these questions, requiring that the analyses are made on returned samples rather than in situ.
3. Background
InformaAon
What
addiAves
are
used?
MulAlayer
films?
PrinAng
Inks?
Which
surfaces
does
the
product
contact?
Are
there
interacAons
between
components?
Is
there
opportunity
for
non-‐product
contact
components
to
migrate?
Are
there
any
processing
aids
used?
3
Materials
of
Construction
Finished
Packaging
4. Use
CondiAons
Extractables
challenge
the
use
condi/on
• Temperature
• Solvent
Strength
• Time
Leachables
mimic
the
most
stringent
use
condi/on
4
How
will
it
be
used?
How
should
it
be
extracted?
5. ExtracAon
Strategies
MulAlayer
Films
Cap
Liners
Printed
Packaging
Containers
based
on
Homo-‐
polymers
Irregularly
shaped
Large
containers
Cut
and
Cover
ExtracAon
Cut
and
Cover
Extraction
Simple
systems
Irregularly
shaped
ArAcles
requiring
two-‐sided
extracAon
Very
large
containers
5
6. ExtracAon
Strategies
MulAlayer
Films
Cap
Liners
Printed
Packaging
Full
Fill
Extraction
MulAlayer
Films
Printed
Packaging
Bags
Small
containers
Tubing
Non-‐
permeable
Printed
containers
6
7. ExtracAon
Strategies
MulAlayer
Films
Cap
Liners
Printed
Packaging
MulAlayer
Films
Printed
Packaging
One-‐Sided
Extraction
MulA-‐layer
Printed
materials
Coated
materials
Product
contacts
one
side
7
8. ExtracAon
Strategies
MulAlayer
Films
Cap
Liners
Printed
Packaging
MulAlayer
Films
Printed
Packaging
Flow
Through
Extraction
Tubing
Complex
systems
In-‐Line
filters
Connectors
8
9. ExtracAon
Strategies
MulAlayer
Films
Cap
Liners
Printed
Packaging
MulAlayer
Films
Printed
Packaging
Large
Volume
Dynamic
Headspace
Direct
analysis
of
the
enAre
arAcle
Very
high
sensiAvity
No
risk
of
volaAles
loss
9
10. ExtracAon
Solvent
Expected
Extractable Type Log
P Boiling
point
Erucamide Hydrophobic 8.8 474
°C
Linear
Alkanes Hydrophobic 8.859 250-‐400
°C
Dibutylphthalate Hydrophobic 4.72 340
°C
Dimethoxyethane VolaAle -‐0.2 85
°C
Irganox
1010 Non-‐volaAle 23 N/A
Irgafos
168 Non-‐volaAle 15.5 N/A
Tinuvin
770 Basic 6.3 N/A
Stearic
acid Acidic 8.23 361
°C
Sodium
benzenesulfonate
Anionic
N/A
N/A
From
the
background
informaAon
provided
for
a
container
closure
system
the
probable
extractables
were:
10
11. Effect
of
Solvent
Polarity
Agilent
1290
Infinity
UHPLC;
Agilent
6520
QTOF-‐MS
Column:
Agilent
Zorbax
Eclipse
Plus
C8;
1.8
µm,
2.1×50
mm
Electrospray
IonizaAon
(ESI);
Polarity:
posiAve
11
12. Extract
PreparaAon
Example:
• 250
mL
per
bag
• Worst
case
3
bags
per
day
• Product
contact
surface
area
310
cm2
• Safety
concern
threshold
(SCT)
=
0.15µg/
day
𝐴𝐸𝑇(µμ 𝑔/𝑏𝑎𝑔 )=0.15 µμ 𝑔∕𝑑𝑎𝑦 /3
𝑏𝑎𝑔𝑠∕𝑑𝑎𝑦 =0.05µμ 𝑔/𝑏𝑎𝑔
𝐸𝑥𝑡𝑟𝑎𝑐𝑡 𝑉𝑜𝑙. (𝑚𝐿)= 310 𝑐 𝑚↑2 /6
𝑐𝑚↑2 ∕𝑚𝐿 =52 𝑚𝐿
𝐿𝑂𝐷=0.05 µμ 𝑔∕𝑏𝑎𝑔 /52 𝑚 𝐿∕𝑏𝑎𝑔
≈1 𝑛 𝑔∕𝑚𝐿
12
14. ConcentraAon
of
Extracts
Extractables
&
Leachables
can
be
lost
during
concentration
Loss
depends
on
• VolaAlity
of
the
analyte(s)
• Extract
handling
Best
PracAces
• Mild
condiAons
• Method
validaAon
• Headspace
analysis
14
21. IdenAficaAon
of
Unknowns
21
Database
Searches
Commercial
Databases
(NIST,
Wiley)
Jordi
Proprietary
AddiAve
and
Oligomer
Databases
QTOF-‐GC
/
QTOF-‐LC
Molecular
Formula
GeneraAon
(MFG)
MS/MS
for
QTOF
-‐LCMS
CI
for
QTOF-‐GCMS
22. IdenAficaAon
of
Unknowns
m/z
Best
Match
Species
Mass
Score
(MFG)
Diff.
(ppm)
DBE
274.2731
C16
H35
N
O2
[M+H]+
273.2660
94.66
2.73
0
22
23. IdenAficaAon
of
Unknowns
Fragment
Ion Best
Match Score Possible
Structure
256.2648
[C16
H34
N
O]+
97.5
230.2496
[C14
H32
N
O]+
84.16
106.0869
[C4
H12
N
O2]+
99.07
88.0764
[C4
H10
N
O]+
99.09
23
24. QuanAtaAve
Strategies
• QuanAficaAon
of
compounds
observed
is
performed
against
surrogate
standards
• Accuracy
depends
on
the
surrogate
standard
used
𝐸𝑠𝑡𝑖𝑚𝑎𝑡𝑒𝑑 𝐴𝑛𝑎𝑙𝑦𝑡𝑒 𝐶𝑜𝑛𝑐.= 𝑂 𝑏𝑠𝑒𝑟𝑣𝑒𝑑 𝐴𝑛𝑎𝑙𝑦𝑡𝑒 𝑃𝑒𝑎𝑘 𝐴𝑟𝑒𝑎/𝑆𝑢𝑟𝑟𝑜𝑔𝑎𝑡𝑒 𝑃𝑒𝑎𝑘 𝐴𝑟𝑒𝑎
× 𝑆𝑢𝑟𝑟𝑜𝑔𝑎𝑡𝑒 𝐶𝑜𝑛𝑐.
Relative
Quantitation
24
26. QuanAtaAve
Strategies
Methodologies:
– External
StandardizaAon
– Standard
AddiAon
Requires
high
purity
analyAcal
standards
Formal
Quantitation
26
Confirmed
compounds
are
quanAfied
against
an
analyAcal
standard
at
a
series
of
concentraAons