Total workflow solutions that cater every budget, performance or throughput requirement for confirmatory dioxin analysis were discussed in the Thermo Scientific Lunch Seminar at the Dioxin 2014 conference. D. Hope, CEO & Owner Pacific Rim Laboratoris, presented about the economies of POPs analysis from the point of view of a leading laboratory using the very latest dioxin method kits. C. Cojocariu, Thermo Fisher Scientific, discussed recent changes in EU regulations which bring new opportunities for more labs to participate in dioxin analysis and about validating methods using Gas Chromatography triple quadrupole for PCDD/Fs with reference to the new EU Commission Regulation No. 709/2014.
Bottom-up workflows have been a staple of mass spectrometry based proteomic approaches. We present in this work a fully automated solution for MALDI-TOF MS based peptide mapping experiments.
EPA Method 200.7, Trace Elements in Water, Solids, and Biosolids by Inductively Coupled Plasma-Atomic Emission Spectrometry, describes the procedure and requirements for multi-element determinations by ICP-AES. This presentation demonstrates the capability of the ICPE-9820, with the ASC-9800 Auto-sampler and the Standard Addition Kit, to produce quick, accurate results that comply with the method.
Total workflow solutions that cater every budget, performance or throughput requirement for confirmatory dioxin analysis were discussed in the Thermo Scientific Lunch Seminar at the Dioxin 2014 conference. D. Hope, CEO & Owner Pacific Rim Laboratoris, presented about the economies of POPs analysis from the point of view of a leading laboratory using the very latest dioxin method kits. C. Cojocariu, Thermo Fisher Scientific, discussed recent changes in EU regulations which bring new opportunities for more labs to participate in dioxin analysis and about validating methods using Gas Chromatography triple quadrupole for PCDD/Fs with reference to the new EU Commission Regulation No. 709/2014.
Bottom-up workflows have been a staple of mass spectrometry based proteomic approaches. We present in this work a fully automated solution for MALDI-TOF MS based peptide mapping experiments.
EPA Method 200.7, Trace Elements in Water, Solids, and Biosolids by Inductively Coupled Plasma-Atomic Emission Spectrometry, describes the procedure and requirements for multi-element determinations by ICP-AES. This presentation demonstrates the capability of the ICPE-9820, with the ASC-9800 Auto-sampler and the Standard Addition Kit, to produce quick, accurate results that comply with the method.
Outline of presentation:
Overview — Plating Baths and High Pressure Liquid Chromatography (HPLC)
Determination of Accelerator and Suppressor by HPLC and Charged Aerosol Detection
Sample Preparation, Calibration, Measurements
Comparisons to CVS data
Determination of Accelerator and Leveller by HPLC and Electrochemical Detection (ECD)
Coulometric Detection Mechanism and Design
Calibration and Measurements
Nickel Additives, Saccharin and Sodium Alkylsulfate
Gage Study Results
Development and validation of hplc method for determination of theophylline a...IJSIT Editor
A stable, simple, rapid, precise, accurate HPLC method for analysis of Theophyllinee and 1-Methyl
Uric Acid was developed and validated as per ICH guidelines without need of any internal standard.
Separation was carried out using X’terra RP18 (250*4.6) mm, 5µ column with potassium dihydrogen
orthophosphate buffer (pH 3): acetonitrile (30:70 v/v) as mobile phase with flow rate 1 mL min-1. The
parameters studied were retention time, linearity and range, accuracy, precision. The proposed method can
be used for determination of Theophylline and 1-Methyl Uric Acid from Human plasma.
A single chromatographic method was developed for the separation and quantitation of ten common seized drugs. The single quadrupole mass spectrometer, LCMS 2020, demonstrated its capability for simultaneous detection and confirmation using in source fragmentation of all analytes. Linear calibration curves were acquired for each analyte.
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
Application of ICP-MS and LC-ICP-MS in Drug DevelopmentQPS Holdings, LLC
Inductively coupled mass spectroscopy plasma (ICP-MS) has big potential in preclinical and clinical studies of new drug candidates. One particular area is metallodrugs.
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.
An introduction to the use of ICP-MS in the clinical setting, that goes on to describe some potential new application areas for advanced instrumentation such as HPLC-ICP-MS, laser ablation-ICP-MS and immuno-tagging-ICP-MS for the measurement of biomolecules.
In this study, a new Shimadzu electrolytic suppressor was used as part of a Shimadzu modular IC system to determine inorganic anions according to methods EPA 300.
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
The growth of, and the confidence in, hemp products will require applicable testing to ensure product quality and safety. Chromatography technology will play a large role in this as the technique is used for potency testing. This study optimizes a quantitative chromatographic determination of 15 cannabinoids using the Shimadzu Hemp Analyzer.
There is high demand for oxysterol quantitation due to their correlation with neurodegenerative diseases. The ratios of various oxysterols in biological fluids are used by researchers to study disease states. This application presents a fast, sensitive LC-MS/MS method using the LCMS-8060, with detection quantitation limits determined using multiple reaction monitoring mode for each analyte.
Validation and Uncertainty Analysis of a Multiresidue Method for
67 Pesticides in Made Tea, Tea Infusion, and Spent Leaves Using Ethyl Acetate Extraction and Gas Chromatography/Mass Spectroscopy
This application note describes the methodology and use of the Shimadzu ICPMS-2030 ICP mass spectrometer for the analysis of trace elements in drinking and fresh waters following the EPA 200.8 method. This method is also used for analysis of wastewater. Here, we demonstrate the stability and sensitivity of the ICPMS-2030 for EPA 200.8 analyses.
Outline of presentation:
Overview — Plating Baths and High Pressure Liquid Chromatography (HPLC)
Determination of Accelerator and Suppressor by HPLC and Charged Aerosol Detection
Sample Preparation, Calibration, Measurements
Comparisons to CVS data
Determination of Accelerator and Leveller by HPLC and Electrochemical Detection (ECD)
Coulometric Detection Mechanism and Design
Calibration and Measurements
Nickel Additives, Saccharin and Sodium Alkylsulfate
Gage Study Results
Development and validation of hplc method for determination of theophylline a...IJSIT Editor
A stable, simple, rapid, precise, accurate HPLC method for analysis of Theophyllinee and 1-Methyl
Uric Acid was developed and validated as per ICH guidelines without need of any internal standard.
Separation was carried out using X’terra RP18 (250*4.6) mm, 5µ column with potassium dihydrogen
orthophosphate buffer (pH 3): acetonitrile (30:70 v/v) as mobile phase with flow rate 1 mL min-1. The
parameters studied were retention time, linearity and range, accuracy, precision. The proposed method can
be used for determination of Theophylline and 1-Methyl Uric Acid from Human plasma.
A single chromatographic method was developed for the separation and quantitation of ten common seized drugs. The single quadrupole mass spectrometer, LCMS 2020, demonstrated its capability for simultaneous detection and confirmation using in source fragmentation of all analytes. Linear calibration curves were acquired for each analyte.
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
Application of ICP-MS and LC-ICP-MS in Drug DevelopmentQPS Holdings, LLC
Inductively coupled mass spectroscopy plasma (ICP-MS) has big potential in preclinical and clinical studies of new drug candidates. One particular area is metallodrugs.
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.
An introduction to the use of ICP-MS in the clinical setting, that goes on to describe some potential new application areas for advanced instrumentation such as HPLC-ICP-MS, laser ablation-ICP-MS and immuno-tagging-ICP-MS for the measurement of biomolecules.
In this study, a new Shimadzu electrolytic suppressor was used as part of a Shimadzu modular IC system to determine inorganic anions according to methods EPA 300.
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
The growth of, and the confidence in, hemp products will require applicable testing to ensure product quality and safety. Chromatography technology will play a large role in this as the technique is used for potency testing. This study optimizes a quantitative chromatographic determination of 15 cannabinoids using the Shimadzu Hemp Analyzer.
There is high demand for oxysterol quantitation due to their correlation with neurodegenerative diseases. The ratios of various oxysterols in biological fluids are used by researchers to study disease states. This application presents a fast, sensitive LC-MS/MS method using the LCMS-8060, with detection quantitation limits determined using multiple reaction monitoring mode for each analyte.
Validation and Uncertainty Analysis of a Multiresidue Method for
67 Pesticides in Made Tea, Tea Infusion, and Spent Leaves Using Ethyl Acetate Extraction and Gas Chromatography/Mass Spectroscopy
This application note describes the methodology and use of the Shimadzu ICPMS-2030 ICP mass spectrometer for the analysis of trace elements in drinking and fresh waters following the EPA 200.8 method. This method is also used for analysis of wastewater. Here, we demonstrate the stability and sensitivity of the ICPMS-2030 for EPA 200.8 analyses.
Lab talk 190210 efficacy studies on radioligand hits_beginnings of fret assay...Laurence Dawkins-Hall
1. Titration of REL 1 antagonist hits identified by radio mimetic assay to quantify efficacy (IC50)
2. Exposition of HT FRET assay principles for large scale compound library screens to empirically identify REL 1 antagonist hits
Part A: To developed analytical (UV) method for determination of TOPIRAMATE in bulk and in oral solid dosage form.
Part B: To validate developed method as per ICH guidelines for parameters:
COLORIMETRY
It is the science & technology used to quantify & describe physically the Human color perception.
selection of drug
1. Drugs which not have strong UV absorbance.
2. Drugs for which Colorimetric methods are not available.
3. Drugs for which methods are available but they are time consuming & complex.
Eg. Dicloxacillin, Topiramate etc.
conclusion
Colorimetric method was developed and validated as per ICH guidelines for estimation of Topiramate in tablets.
Development of color is by reaction of amino group of drug with Ninhydrin reagent in presence of pyridine.
The method was found to be simple, accurate, precise and specific.
So, the proposed method can be used for the routine quality control analysis of the bulk drug as well as oral dosage forms.
Measuring Comparability of Conformation, Heterogeneity and Aggregation with C...KBI Biopharma
"Measuring Comparability of Conformation, Heterogeneity, and Aggregation with Circular Dichroism and Analytical Ultracentrifugation", invited talk, State of the Art Methods for the Characterization of Biological Products and Assessment of Comparability, NIH, June 2003
Quantitative Analysis of Oligonucleotides in Human Muscle Tissue Using Liquid...Covance
APA 2019 -- Duchenne muscular dystrophy (DMD) is a rare X-linked recessive neuromuscular disease characterized by progressive severe muscle wasting and weakness. DMD is ultimately fatal, with patients typically dying from respiratory or cardiac complications in their mid- to late-20s. Exon skipping by phosphorodiamidate morpholino oligomer (PMO) is considered a promising, disease-modifying approach to treat the underlying cause of DMD. PMO was conjugated to a proprietary peptide to enhance tissue uptake, providing a PPMO. This poster describes the development and validation of a sensitive, selective and high-throughput liquid chromatography-tandem high resolution-accurate mass (LC/HR-AM) method for the quantitation of the PPMO in human muscle tissue using an analogue as the internal standard (ISTD). A key modification to the PMO is the addition of a proprietary peptide that provides specificity to binding and due to the metabolism of the peptide several entities of the PMO will be present in the muscle tissue, in order to quantitate the total amount of the PPMO in the muscle. The extraction undergoes a peptide digestion step to form an end product of PMO-A prior to the analysis.
Development and validation of a stability-indicating HPLC method for the simultaneous determination of Losartan potassium, hydrochlorothiazide, and their degradationproducts
UHPLC has proven to be an effective way to reduce analysis times without losing separation efficiency through the use of small particle and core-shell column technologies. The use of higher column temperatures and shorter column lengths has allowed the analysis speed of UHPLC to be further increased. A number of high-speed UHPLC applications and conditions will be presented which now allow up to four analytical runs to be completed in only a one-minute timeframe.
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
Combination drugs containing Paracetamol and Aspirin, displayed in Figure 1, are widely used analgesics with anti-inflammatory properties for treatment of migraines. Both active ingredients have a similar mode of action, whereby they inhibit the cyclooxygenase (COX) enzyme, by preventing the production of prostaglandins which cause pain, inflammation, and fever. UV/Vis spectrometry is a fast and commonly used technique in quality control laboratories for routine analysis of purity and quantity of components within various stages of a product’s manufacture in many industries.
Francesca Gottschalk - How can education support child empowerment.pptxEduSkills OECD
Francesca Gottschalk from the OECD’s Centre for Educational Research and Innovation presents at the Ask an Expert Webinar: How can education support child empowerment?
2024.06.01 Introducing a competency framework for languag learning materials ...Sandy Millin
http://sandymillin.wordpress.com/iateflwebinar2024
Published classroom materials form the basis of syllabuses, drive teacher professional development, and have a potentially huge influence on learners, teachers and education systems. All teachers also create their own materials, whether a few sentences on a blackboard, a highly-structured fully-realised online course, or anything in between. Despite this, the knowledge and skills needed to create effective language learning materials are rarely part of teacher training, and are mostly learnt by trial and error.
Knowledge and skills frameworks, generally called competency frameworks, for ELT teachers, trainers and managers have existed for a few years now. However, until I created one for my MA dissertation, there wasn’t one drawing together what we need to know and do to be able to effectively produce language learning materials.
This webinar will introduce you to my framework, highlighting the key competencies I identified from my research. It will also show how anybody involved in language teaching (any language, not just English!), teacher training, managing schools or developing language learning materials can benefit from using the framework.
Welcome to TechSoup New Member Orientation and Q&A (May 2024).pdfTechSoup
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Honest Reviews of Tim Han LMA Course Program.pptxtimhan337
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Unit 8 - Information and Communication Technology (Paper I).pdfThiyagu K
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Macroeconomics- Movie Location
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Prepare a presentation or a paper using research, basic comparative analysis, data organization and application of economic information. You will make an informed assessment of an economic climate outside of the United States to accomplish an entertainment industry objective.
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3. Challenge
Goal: To identify and quantitate the main
ingredient in a low dose nasal formulation.
Bonus: To identify and quantitate other
constituents in the formulation.
Materials Provided: 7 x 125 µL sample units and
2 x 125 µL placebo units of the formulation.
3
5. Identification by MS
• Components identified by a series of high and
low resolution mass spectrometry
experiments
• MS data was acquired using a Bruker Solarix
XR mass spectrometer in positive electrospray
mode
• The structure elucidation predictions made by
High (XRMS) and Low (SQD) resolution MS are
consistent and exactly overlap with the
structure of Hydrocortisone 5
9. NMR
• Instrument: Bruker-Biospin AVANCE III NMR
spectrometer operating at 600 MHz
• Solvent: DMSO-d6 with TMS as NMR reference
and Maleic Acid as internal standard
• Compared HNMR spectrum of Hydrocortisone
Standard versus the formulation
9
11. Identification of Other
Components
• Identified other components by LC-MS
• LCMS helped establish the structure of four
other constituents
• Main component Hydrocortisone – likelihood
that other components were related to it.
• The four other constituents were identified by
MS and confirmed by literature search
11
13. Other Components
1) Cortisone
• A m/z 361.3 was obtained for the peak at RT 2.639 min.
• The UV spectrum for this peak is similar to that of
hydrocortisone, which suggested it, was a closely related
steroidal compound.
• Cortisone has a mass of 360.4 (which is consistent with m/z
361.3) and is a common degradation product of
Hydrocortisone.
• This constituent was then confirmed to be Cortisone by
comparing its RT to the RT of a Cortisone standard obtained
from the market.
13
15. Other Components
2) Prednisone
• A m/z 359.2 was obtained for the peak at RT 2.429
min.
• The UV spectrum for this peak is similar to that of
hydrocortisone and cortisone, which suggested it,
was a closely related steroidal compound.
• Prednisone has a mass of 358.4 (which is consistent
with m/z 359.2).
• This constituent was then confirmed to be
Prednisone by comparing its RT to the RT of a
Prednisone standard.
15
16. Other Components
3) Prednisolone/21-al impurity
• A m/z 361.2 was obtained for the peak at RT 3.057 min.
• The UV spectrum for this peak is similar to that of
hydrocortisone, which suggested it, was a closely related
steroidal compound.
• Two possibilities:
1) The 21-aldehyde derivative of hydrocortisone - mass of 360.2
(which is consistent with m/z 361.2) and is a common
degradation product of Hydrocortisone. Seen in
Hydrocortisone Standard as well!
2) Prednisolone – also has a mass of 360.4 (which is
also consistent with m/z 361.2)
16
22. 4) Polyethylene Glycol
• The characteristic umbrella pattern is typical
of polyethylene glycol molecules.
• The MS pattern shows fragments that are 44
mass units apart, which also confirms the
presence of PEG.
• The masses are around the range of 400 Da,
which confirmed that this component was
PEG 400.
22
24. Dissolving Solvent
• In-silico prediction tool “Cosmotherm”
• Highly hydrophobic neutral compound with some polar
groups
• Good solubility in organic solvents such as Ethanol, Methanol,
THF, and 50/50 mixtures of aqueous and organic solvents
• Explored different ratios of Ethanol/Water (30/70 and 50/50)
and Methanol/Water (50/50) and also Acetonitrile/Water
(50/50)
• Relatively low solubility in Acetonitrile
• Chosen dissolving solvent: 50/50 mixture of Ethanol/Water
24
26. Achiral UPLC Screen
26
System Used: Waters Acquity with PDA detector and solvent switcher
Time %Buffer %Acetonitrile Flow Rate: 0.5 ml/min
0.00 95 5 Column Temp: 45° C
8.2 0 100 Inj Vol: Varies from 1-5 μl
8.7 0 100 Detection: UV-210 nm (200-400 nm collected)
8.8 95 5 (10pts/sec with 4.8 nm bandwidth)
10.30 95 5
Method Buffer Column
1 50mM Sodium Perchlorate Waters BEH C8 2.1 x 100mm 1.7 um
With 0.1% Phosphoric Acid
(pH ~2.1)
2 10mM Ammonium Bicarbonate Waters BEH C8 2.1 x 100mm 1.7 um
(pH ~8.0)
3 0.1% Methanesulfonic Acid Waters BEH RP C18 2.1 x 100 mm 1.7 um
(pH ~2)
4 0.1% Methanesulfonic Acid Waters HSS T3 2.1 x 100 1.8 um
(pH ~2)
27. Not Good Enough!
• None of the screening methods was able to efficiently
separate the components.
• All the screening methods utilized Acetonitrile as the organic
portion of the mobile phase.
• Since all of the components are steroidal in nature, there is a
high degree of hyrophobicity associated with them.
• Replaced Acetonitrile with a stronger organic solvent.
• A 2:1 mixture of THF and Methanol was used as the organic
portion of the mobile phase. Different proportions of aqueous
to organic were evaluated to obtain the best
chromatographic profile
27
28. Optimized Chromatographic
Conditions
CHROMATOGRAPHIC CONDITIONS
Chromatographic system: Waters Acquity UPLC
Column: RP shield C18, 1.8 µm, 2.1 x 100 mm
Column Temperature: 45 °C
Injection Volume: 2 uL
Flow Rate: 0.4 mL/min
Detection: UV @ 245 nm
Mobile Phase:
Isocratic
A (77%):
0.05% MSA in Water
B (23%):
THF:Methanol (2:1)
Dissolving Solvent: Ethanol : Water (50:50)
Run-Time 4.0 min
28
29. Validation Parameters
Parameter Method Result
Linearity 0.05mg/ml- 0.13mg/ml) R² = 1.0
LOQ 0.3% of nominal Recovery = 91%
System Precision 5 injections at nominal
(0.08mg/ml)
RSD = 0.8%
Method Precision 3 Assays of Sample RSD = 3.9%
Solution Stability
(Standard and Sample)
24 hour time point Std recovery= 100.2%
Spl recovery= 98.9% of
initial time point
29
32. Quantitation Protocol
• After successfully validating, and comparing sample responses
to the curve, nominal concentration for Hydrocortisone was
set at 0.08mg/mL
• Cortisone Standard: Prepared a standard of Cortisone at
0.002678 mg/ml
• Prednisone Standard: Prepared a standard of Prednisone at
0.002312 mg/ml
• Prednisolone was quantitated against hydrocortisone
standard.
• Quantitation was performed by preparing 3 individual samples
• Samples were prepared by diluting about 100mg of
formulation in 1ml volumetric flasks to obtain area responses
comparable to that of the standard at nominal concentration.32
34. Comparison with USP Method
Comparison CoSMoS Method USP Method
Instrument time 4.0 min per injection 15.0 min per injection
Organic solvent
consumption per sample
0.5mL per sample 1mL per sample
Organic solvent
consumption per injection
0.37mL 7.5mL
Cost of column $400 $400
Total Time Say “T” Approx “4T”
Total Cost Say “C” Approx “ 20C”
34
36. Conclusion
• The main component of the low dose formulation was identified
to be Hydrocortisone (by HRMS and NMR)
• Six out of the Nine components were identified and quantitated
• Simplified sample preparation
A simple dissolving solvent Water/Ethanol (50/50)
Short sample preparation time
• Rapid UHPLC method for Quantitation
Reduced run-time on the instrument within 4.0 min
Highly cost effective
Accurate and Precise
Green
36