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.
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of gas chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical points of the method, assisting analysts in modifying existing methods, and understanding instrumental and software technologies with the goal of improving laboratory productivity and reducing the overall cost per sample. The results of experiments for both screening and quantification workflows, using the latest technology, will be presented.
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical aspects of the method, assisting analysts in optimizing their methods for the most challenging analyses.
Key Learning Objectives
- Learn how the use of automated software can make SRM development faster and more highly optimized.
- Learn how the use of a compound data store can further simplify method creation.
- Learn how the use of retention time-based SRM acquisition can increase MS/MS sensitivity and make method maintenance easier.
Event Overview:
In recent years, Gas Chromatography-triple quadrupole mass spectrometry has increased in popularity due to its ability to offer lower detection limits in complex matrices, simplified sample prep requirements, and faster analysis times. Of course, new instrument technology presents the need for the acquiring of new skills to harness the advantages offered by its adoption into current workflows.
In this webinar, a strategy for addressing both of these challenges is discussed in the context of new software designed to automate common method development and method maintenance tasks. Also, in addition to making the triple quadrupole easier to use, this strategy can increase sensitivity of the analysis, which will be demonstrated using a complex SRM pesticide method as an example.
For more information: www.thermoscientific.com/tsq8000
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.
This webinar will provide pesticides residue analysts with valuable information on software method development and data processing for the analysis of pesticide residues in food for both LC–MS and GC–MS. Technical experts will review the latest in software advances to help with data interpretation and reporting.
The presentation describes the automated process of the system and present a number of applications from sample matrices such as food, polymers, and pharmaceuticals to show the utility of the system.
Recently, a new technique was introduced the allows the automated supercritical extraction and SFC analysis of samples with minimal sample preparation and handling requirements to save analyst time and sample preparation expenses. This presentation demonstrates how automated SFE-SFC can be a quick way to screen up to 48 soil samples for explosives in a variety of soil types with minimal sample prep. For more information, go to http://www.ssi.shimadzu.com/industry/industrypage.cfm?market_id=4. Thanks for viewing.
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of gas chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical points of the method, assisting analysts in modifying existing methods, and understanding instrumental and software technologies with the goal of improving laboratory productivity and reducing the overall cost per sample. The results of experiments for both screening and quantification workflows, using the latest technology, will be presented.
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical aspects of the method, assisting analysts in optimizing their methods for the most challenging analyses.
Key Learning Objectives
- Learn how the use of automated software can make SRM development faster and more highly optimized.
- Learn how the use of a compound data store can further simplify method creation.
- Learn how the use of retention time-based SRM acquisition can increase MS/MS sensitivity and make method maintenance easier.
Event Overview:
In recent years, Gas Chromatography-triple quadrupole mass spectrometry has increased in popularity due to its ability to offer lower detection limits in complex matrices, simplified sample prep requirements, and faster analysis times. Of course, new instrument technology presents the need for the acquiring of new skills to harness the advantages offered by its adoption into current workflows.
In this webinar, a strategy for addressing both of these challenges is discussed in the context of new software designed to automate common method development and method maintenance tasks. Also, in addition to making the triple quadrupole easier to use, this strategy can increase sensitivity of the analysis, which will be demonstrated using a complex SRM pesticide method as an example.
For more information: www.thermoscientific.com/tsq8000
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.
This webinar will provide pesticides residue analysts with valuable information on software method development and data processing for the analysis of pesticide residues in food for both LC–MS and GC–MS. Technical experts will review the latest in software advances to help with data interpretation and reporting.
The presentation describes the automated process of the system and present a number of applications from sample matrices such as food, polymers, and pharmaceuticals to show the utility of the system.
Recently, a new technique was introduced the allows the automated supercritical extraction and SFC analysis of samples with minimal sample preparation and handling requirements to save analyst time and sample preparation expenses. This presentation demonstrates how automated SFE-SFC can be a quick way to screen up to 48 soil samples for explosives in a variety of soil types with minimal sample prep. For more information, go to http://www.ssi.shimadzu.com/industry/industrypage.cfm?market_id=4. Thanks for viewing.
Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. In cleaning validation protocols, direct sampling is performed with swabs, which are sticks with textiles at one end. The sample on the swab after swabbing the surface of equipment is analyzed with a TOC analyzer and HPLC. Recently, HPLC has been more preferable because of the growing need for the individual analysis of products. Before the HPLC analysis, manual processes such as a sample extraction and a sample condensation are required. Such manual processes may affect to the quality of results. Thus, we evaluated the application of a novel on-line supercritical fluid extraction/chromatography system for the cleaning validation.
For more information, go to ssi.shimadzu.com and follow us on Twitter @ShimdzuSSI
Fast, selective, and sensitive methods can be developed for the analysis of impurities
Offering many business benefits using UPLC and UPC2
Increase in sample throughput
Reduction in toxic solvent usage
Using mass spectral detection over UV detection provides
Improvement in sensitivity and selectivity
Reduced matrix effects
PDA and mass detection provide complementary information for peak assignment and structural confirmation of impurities
Learn about Waters technologies for analyzing oligonucleotides with LC-MS. We offer solutions for both oligo characterization and QC monitoring. Learn more: http://www.waters.com/oligos
Determination of Carbohydrates in Various Matrices by Capillary High-Performance Anion-Exchange Chromatography with Pulsed Amperometric Detection (HPAE-PAD)
This presentation describes the combined advantages of a reagent-free capillary format Ion Chromatography (IC) to determine monosaccharides and disaccharides in various applications, from low concentrations in synthetic urine samples to high concentrations in beverage samples. In a reagent-free IC system, the hydroxide eluent is electrolytically generated inline to deliver accurate and precise concentrations for isocratic or gradient separations by only adding deionized water. Eluent generation eliminates carbonate contamination and errors from manual preparation. A capillary scale system with µL/min flow rates can run 24/7, always on and always ready for samples.
High-performance anion-exchange chromatography with pulsed amperometric detection is valuable for oligosaccharide analysis with the value derived from the high-resolution separation followed by sensitive detection of native oligosaccharides. In this presentation the application of HPAE-PAD to oligosaccharides released from glycoproteins is demonstrated.
The webinar is all about Ultra High Pressure Liquid Chromatography (UHPLC) performance and how new column technology can deliver the best separation power and be married with the best UHPLC system to ensure an outstanding result. It covers how chromatographers can ensure that even very complex and unfamiliar samples are assayed with the highest scrutiny possible? The webinar discusses how to get the most out of solid core column technology with the right UHPLC system. It covers the use of an extremely long column approach for ultra-high resolution assays and the outlines the importance of robustness and retention time stability.
Industrial Laboratories around the world are trying to find ways to minimize sample preparation and enhance productivity. The adaptation of modern mass spectrometry instrumentation is desired due to the high sensitivity and selectivity they provide. This presentation will describe how different sample preparation techniques can be simplified and automated for LC/MS/MS analyses.
Key Learning Objectives:
- Identify the biggest time-consuming activities that occur in the Gas Chromatography-Mass Spectrometry (GC-MS) workflow
- Learn a modern approach to minimize the time an operator spends on the data review, reporting, and complex method development
Overview:
In the routine workflow of daily GC-MS operations, analysts spend the majority of their workday reviewing data and conducting maintenance activities. Today, many laboratories are also exploring the addition of MS/MS capabilities. Add the MS/MS dimension along with more complex method development to this workflow, and the analyst’s workload becomes even more challenging.
How can we mitigate this challenge? In this web seminar, we will demonstrate how the efficiency of data analysis can be improved through dynamic, interactive GC-MS data review and automated MS/MS method development. Additionally, we will illustrate some innovative ways to minimize downtime on the instrument for maintenance activities, whether planned or unplanned, to help alleviate this burden on the analyst. Common challenges and corresponding solutions will be presented throughout.
For more information: http://www.thermoscientific.com/isq
Overview of webinar:
Rechargeable, manganese-based, lithium-ion batteries (LiBs) are environmentally friendly, have a good safety record, and can be made at a lower cost than other metal-based LiBs. However, they have a shorter lifetime. Much research has been spent on improving product safety, cycle life, and product performance, yet understanding fundamental processes and degradation mechanism in LiBs remains a challenge. Identifying breakdown products and understanding degradation processes can lead to enhancing battery performance, improvements in product safety, and insight into component failure mechanisms.
This presentation evaluates ASTM D7979-16 for the “direct” analysis of 30 PFCs and compares data to the solid-phase extraction EPA drinking water Method 537.
The feature of the new general chapter 621 is that a column packed with small particles can be used if column length and particle ratio (L/dp) is kept constant between the designated and modified column. This enables high speed analysis of USP methods more than ever.
In this study, a USP method was successfully transferred to an ultra-high speed method with the system suitability requirements met.
For more information, go to SSI.Shimadzu.com. Thanks for viewing.
Simplifying Chromatographic Methods Transfer: Novel Tools for Replicating You...Waters Corporation
Gain a good understanding on the parameters that impact the successful transfer of an LC method from one instrument to another as well as some of the novel tools (i.e., Arc Multi-flow path technology and gradient SmartStart) that have been created to enable the ACQUITY Arc System to replicate established HPLC methods from previous generations of LC equipment.
Transfer of established gradient reversed-phase methods across both HPLC and UHPLC chromatographic instrumentation requires careful consideration of each instrument’s operating parameters and design. The dwell volume, or the system volume between when the solvents are first mixed and the head of the column, can impact the separation. In addition to the dwell volume, the manner in which the solvents are mixed and the formation of the gradient can also vary from one type of LC system to another. Finally, the manner in which the column and solvent are heated can also effect the separation, specifically whether or not the solvent is passively or actively heated prior to the column, or if the air is static or circulated within the column oven.
To understand the effect of these factors may have on methods transfer, both method conditions and instrument specifications must be factored and evaluated when transferring an LC method from one instrument to another.
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.
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.
Cleaning validation is necessary to establish the quality and safety of pharmaceutical drug products. In cleaning validation protocols, direct sampling is performed with swabs, which are sticks with textiles at one end. The sample on the swab after swabbing the surface of equipment is analyzed with a TOC analyzer and HPLC. Recently, HPLC has been more preferable because of the growing need for the individual analysis of products. Before the HPLC analysis, manual processes such as a sample extraction and a sample condensation are required. Such manual processes may affect to the quality of results. Thus, we evaluated the application of a novel on-line supercritical fluid extraction/chromatography system for the cleaning validation.
For more information, go to ssi.shimadzu.com and follow us on Twitter @ShimdzuSSI
Fast, selective, and sensitive methods can be developed for the analysis of impurities
Offering many business benefits using UPLC and UPC2
Increase in sample throughput
Reduction in toxic solvent usage
Using mass spectral detection over UV detection provides
Improvement in sensitivity and selectivity
Reduced matrix effects
PDA and mass detection provide complementary information for peak assignment and structural confirmation of impurities
Learn about Waters technologies for analyzing oligonucleotides with LC-MS. We offer solutions for both oligo characterization and QC monitoring. Learn more: http://www.waters.com/oligos
Determination of Carbohydrates in Various Matrices by Capillary High-Performance Anion-Exchange Chromatography with Pulsed Amperometric Detection (HPAE-PAD)
This presentation describes the combined advantages of a reagent-free capillary format Ion Chromatography (IC) to determine monosaccharides and disaccharides in various applications, from low concentrations in synthetic urine samples to high concentrations in beverage samples. In a reagent-free IC system, the hydroxide eluent is electrolytically generated inline to deliver accurate and precise concentrations for isocratic or gradient separations by only adding deionized water. Eluent generation eliminates carbonate contamination and errors from manual preparation. A capillary scale system with µL/min flow rates can run 24/7, always on and always ready for samples.
High-performance anion-exchange chromatography with pulsed amperometric detection is valuable for oligosaccharide analysis with the value derived from the high-resolution separation followed by sensitive detection of native oligosaccharides. In this presentation the application of HPAE-PAD to oligosaccharides released from glycoproteins is demonstrated.
The webinar is all about Ultra High Pressure Liquid Chromatography (UHPLC) performance and how new column technology can deliver the best separation power and be married with the best UHPLC system to ensure an outstanding result. It covers how chromatographers can ensure that even very complex and unfamiliar samples are assayed with the highest scrutiny possible? The webinar discusses how to get the most out of solid core column technology with the right UHPLC system. It covers the use of an extremely long column approach for ultra-high resolution assays and the outlines the importance of robustness and retention time stability.
Industrial Laboratories around the world are trying to find ways to minimize sample preparation and enhance productivity. The adaptation of modern mass spectrometry instrumentation is desired due to the high sensitivity and selectivity they provide. This presentation will describe how different sample preparation techniques can be simplified and automated for LC/MS/MS analyses.
Key Learning Objectives:
- Identify the biggest time-consuming activities that occur in the Gas Chromatography-Mass Spectrometry (GC-MS) workflow
- Learn a modern approach to minimize the time an operator spends on the data review, reporting, and complex method development
Overview:
In the routine workflow of daily GC-MS operations, analysts spend the majority of their workday reviewing data and conducting maintenance activities. Today, many laboratories are also exploring the addition of MS/MS capabilities. Add the MS/MS dimension along with more complex method development to this workflow, and the analyst’s workload becomes even more challenging.
How can we mitigate this challenge? In this web seminar, we will demonstrate how the efficiency of data analysis can be improved through dynamic, interactive GC-MS data review and automated MS/MS method development. Additionally, we will illustrate some innovative ways to minimize downtime on the instrument for maintenance activities, whether planned or unplanned, to help alleviate this burden on the analyst. Common challenges and corresponding solutions will be presented throughout.
For more information: http://www.thermoscientific.com/isq
Overview of webinar:
Rechargeable, manganese-based, lithium-ion batteries (LiBs) are environmentally friendly, have a good safety record, and can be made at a lower cost than other metal-based LiBs. However, they have a shorter lifetime. Much research has been spent on improving product safety, cycle life, and product performance, yet understanding fundamental processes and degradation mechanism in LiBs remains a challenge. Identifying breakdown products and understanding degradation processes can lead to enhancing battery performance, improvements in product safety, and insight into component failure mechanisms.
This presentation evaluates ASTM D7979-16 for the “direct” analysis of 30 PFCs and compares data to the solid-phase extraction EPA drinking water Method 537.
The feature of the new general chapter 621 is that a column packed with small particles can be used if column length and particle ratio (L/dp) is kept constant between the designated and modified column. This enables high speed analysis of USP methods more than ever.
In this study, a USP method was successfully transferred to an ultra-high speed method with the system suitability requirements met.
For more information, go to SSI.Shimadzu.com. Thanks for viewing.
Simplifying Chromatographic Methods Transfer: Novel Tools for Replicating You...Waters Corporation
Gain a good understanding on the parameters that impact the successful transfer of an LC method from one instrument to another as well as some of the novel tools (i.e., Arc Multi-flow path technology and gradient SmartStart) that have been created to enable the ACQUITY Arc System to replicate established HPLC methods from previous generations of LC equipment.
Transfer of established gradient reversed-phase methods across both HPLC and UHPLC chromatographic instrumentation requires careful consideration of each instrument’s operating parameters and design. The dwell volume, or the system volume between when the solvents are first mixed and the head of the column, can impact the separation. In addition to the dwell volume, the manner in which the solvents are mixed and the formation of the gradient can also vary from one type of LC system to another. Finally, the manner in which the column and solvent are heated can also effect the separation, specifically whether or not the solvent is passively or actively heated prior to the column, or if the air is static or circulated within the column oven.
To understand the effect of these factors may have on methods transfer, both method conditions and instrument specifications must be factored and evaluated when transferring an LC method from one instrument to another.
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.
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.
STUDIES ON INTEGRATED BIO-HYDROGEN PRODUCTION PROCESS-EXPERIMENTAL AND MODELINGArghya_D
In the project “Studies on integrated biohydrogen production process-Experimental and Modeling”,a co-culture (mixture of two microorganisms in a single reactor) study of a dark fermentative and photofermentative microorganism was done to assess its hydrogen production performance. For modeling purpose, Artificial Neural Network and Genetic Algorithm has been used as a stochastic technique. The optimized data from batch study was successfully used to run a photobioreactor in continuous mode. A mechanistic model was developed for a continuous co-culture setup using data from literature and solved using MATLAB.
This presentation describes the operation and application of the Waters APGC (Atmospheric Pressure Gas Chromatography) ion source which provides a highly sensitive GC-MS, MS/MS capability for tandem quadrupole and time of flight MS systems. It is very easy to swap between APGC, Electrospray (for UPLC) and other ion sources without instrument venting in minutes.
APGC provides significant performance advantages over traditional GC/MS ionisation methods, giving high sensitivity and less fragmented spectra.
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.
IDNADEX: Improving DNA Data Exchange Validation Studies of a Global STR SystemThermo Fisher Scientific
IDNADEX: Improving DNA Data Exchange
Validation Studies of a Global STR System
Presented by Dr. Antonio Alonso
National Institute of Toxicology and Forensic Sciences, Madrid, Spain
Concluding Remarks:
The data reported demonstrates the GlobalFiler® PCR amplification system followed by
CE detection in a 3500 Genetic Analyzer generates high quality, reproducible, precise,
accurate, and sensitive profiling STR data, even from sub-nanogram amounts of genomic
DNA template and also in the presence of powerful PCR inhibitors co-extracted with
DNA from a high variety of forensic samples including the following DNA sources: blood,
semen & saliva stains, hair, muscle, liver, bone and teeth.
The GlobalFiler® system provides equivalent overall performance to previous forensic STR
PCR kits, but with enhanced discrimination power for a better match efficiency that
would reduce the chance of adventitious matches during DNA data exchange among
national DNA databases.
The use of GlobalFiler® kit would be also very beneficial to improve discrimination power
of DNA analysis not only in criminal DNA databases, but also in many other forensic
applications of autosomal STR profiling including missing person identification, disaster
victim identification, mass grave investigations and kinship analysis.
For this study, 34 pesticides were selected for analysis based on the types of pesticides that are commonly used in MM production. The data presented illustrate how a triple quadrupole GC-MS/MS operated in the MRM mode, can be used to analyze for trace-level pesticide residues in complex plant matrices such as medical marijuana. For more information, go to www.ssi.shimadzu.com. Thanks for viewing!
Cooper Environmental’s Xact® 640 is the first Multi-Metals Continuous Emissions Monitor to be proven successful for accurately measuring elemental concentrations in smoke stacks by capturing and measuring both particulate and vapor phase metals.
Development of a Multi-Variant Frequency Ladder™ for Next Generation Sequenci...Thermo Fisher Scientific
Increasing adoption of NGS has shed light on the need for more
standardized controls to evaluate and optimize system performance.
Samples containing mutations of interest are difficult to source and cell
line pooling experiments to determine limit of detection require significant
investments of time and money. To simultaneously evaluate variant
calling performance in >200 unique amplicons across 50 genes targeted
by NGS tests, AcroMetrix® has developed a proprietary
genomic/synthetic DNA material containing over 550 mutations as a
mixture of SNV’s indels and MNP’s. The limit of detection was then
determined for >400 variants using multiple platforms. Tumor samples
were diluted with matched normal samples to mimic a range of
frequencies. Linearity between the material and diluted tumor tissue
samples were compared. Overall, highly multiplex controls with tunable
frequencies allow for much more extensive, yet streamlined, assay
evaluation and facilitate implementation and impart confidence to NGS
testing.
Presentation by Dr. Sarah Cianférani-Sanglier, University of Strasbourg, Strasbourg, France. Talk given at Waters Antibody Drug Conjugates (ADC) 2014 Meeting, Nov. 20-21, Wilmslow UK.
This presentation will focus on the new USP Chapter <2232> on elemental contaminants in dietary supplements. In particular, it will discuss the permitted daily exposure (PDE) limits of the four heavy metals of toxicological concern defined in the chapter and the different options for measurement strategies to meet these limits. In addition it will give an overview of the new USP Chapter <233>, which describes the suggested sample preparation, instrumental techniques and validation protocols required to demonstrate compliance of the analytical procedure used.
In this webinar Dr. Bertrand Rochat of Faculté de Biologie et de Médecine of the Centre Hospitalier Universitraire Vaudois (CHUV) at Lausanne discusses the paradigm shift to high resolution mass spectrometry (HRMS) in clinical research for quantitative analyses (sensitivity, selectivity, etc.). Quantifications in high resolution full scan or MS/MS mode will be compared with triple quadrupole MS. He will present Quan/Qual analysis with a study on the fate of an anti-cancer agent in human: with over 40 metabolites being identified and quantified; as well as metabolomics data underscoring the versatility of high resolution Orbitrap MS.
Many factors impacting the measurement precision of ICP-OES and ICP-MS are still often neglected for everyday operation, however. Sample preparation is one of the factors that play a crucial role in the success of high-quality sample analysis. In this webinar, our experts will discuss sample preparation to: 1) improve analysis precision 2) make difficult samples easy to be analyzed 3) eliminate sample dilution to minimize error introduction.
For more information, please visit here: http://chrom.ms/CtRtKpw
Join the experts as they discuss the use of accelerated solvent extraction and QuEChERS techniques for the extraction of pesticide residues from a diverse range of food samples. Tips and tricks for improving the extraction efficiency will be covered, along with selection criteria for each technique by sample type, assisting analysts in modifying existing methods or developing new methods to tackle their analytical challenges
In the pharmaceutical arena there is great interest in solid core technology, where there is a broad range of sample types as well as requirements throughout the process of developing new chemical entities. The presentation looks at how solid core technology can be readily adapted to cope with the challenges associated with the pharmaceutical sector, looking at various sample matrices and molecular entities, from small molecules to large biomolecules. The presentation gives an insight into how varying the solid core to porous layer allows the user to optimize separation performance by reducing extra band broadening. Data presented demonstrates how this technology is more robust than fully porous systems when analyzing biological extracts, routinely used in DMPK departments, resulting in longer column lifetimes.
Stationary Phase and Mobile Phase Selection for Liquid Chromatography
The presentation focuses on how to choose the appropriate mode of separation, the correct column and highlights the importance of the correct mobile phase. This approach will be applied to a wide selection of compound types ranging from proteins, peptides, glycans to small pharmaceutical molecules and their metabolites. It will also look at specific application areas for monoclonal antibody analysis, namely: titer, aggregation, charge and oxidation variant. Platform methods for biologics characterization are also discussed.
Investigation into the design and application of solid core stationary phases has led to a better understanding of how the phases work and has resulted in their design aligned to the structure of the analytes being separated. The current range of columns available is discussed both in terms of selectivities, and also morphologies, allowing informed decisions to be made by the chromatographer. Using real life examples, coupled with advanced modeling, the effects of the particle size and morphology will be given for both small and large molecules, offering an insight into what the future holds for solid core products.
Over the past decade, there have been a growing number of mAb candidates entering the clinical pipeline. This results in a large increase on the demand for analytical characterization. This seminar discusses advances in analytical method development with analytical run times below 10 minutes for all routine methods with intelligent, integrated chromatography workflows. Orbitrap technology has been established as the most powerful MS technology for protein characterization. How this can be incorporated into a complete workflow for bio-pharma analysis is also discussed.
Analysis of Disinfection Byproducts by Ion Chromatography
In this presentation, the use of ion chromatography for the determination of bromate, chlorate and haloacetic acids for compliance monitoring according to various ISO standards (15061, 11206, 10304-4, 23631) and U.S. EPA Method 557 will be discussed. Examples will include IC methods using electrolytically generated hydroxide eluents on an RFIC™ system.
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.
Analysis of Anions and Cations in Produced Water from Hydraulic Fracturing Using Ion Chromatography
This presentation describes the use of ion chromatography (IC) to determine anions and cations in produced water from three different hydraulic fracturing sites. Considerable variation in ion concentration was found, which was attributed to differences in the geology of the locations from which samples were obtained.
Analysis of Cations in Hydraulic Fracturing Flowback Water from the Marcellus Shale Using Ion Chromatography
This presentation describes the determination of cations in hydraulic fracturing flowback water using ion chromatography. In this work, sodium was most abundant, followed by calcium, strontium, magnesium, potassium, barium, ammonium, and then lithium, respectively. The quantity of scale-forming ions, such as calcium, strontium, and barium, is particularly informative because it can be used to determine the amount of anti-scaling agent in fracturing fluid mix that will maximize hydrocarbon recovery.
Today’s analytical laboratory is faced with tight deadlines to produce results from testing environmental samples. Too often, solid-phase extraction (SPE) presents a bottleneck in the analytical testing process and may cause poor analyte recoveries and highly variable. Despite advances in analytical instrumentation, sample prep often relies on tedious, manual, and expensive techniques such as liquid-liquid extraction.
Sample preparation of environmental water samples can be automated, however.. Use of automated sample preparation addresses the many challenges that laboratories face when preparing samples and can help improve sample processing turnaround times.
Chromatography presentation goes with this free on-demand webinar. Link to webinar: https://event.on24.com/eventRegistration/EventLobbyServlet?target=registration.jsp&eventid=832348&sessionid=1&key=7401504685427A0804ABBD1F956E617C&partnerrefthermo=undefined&sourcepage=register
The importance of clean drinking water is recognized worldwide. In the U.S., the Environmental Protection Agency (EPA) has established Maximum Contamination Limits (MCL) for monitoring toxic contaminants that may cause adverse health effects. Other ions, such as chloride and sulfate are monitored for aesthetic characteristics under the U.S. National Secondary Drinking Water Standards guidelines. Similar regulations for clean drinking water have been implemented in other industrialized countries. Ion Chromatography (IC) methods have been approved for compliance monitoring including U.S. EPA 300.0 in 1993. Learn about using ion chromatography for the determination of inorganic anions, perchlorate and chromate for compliance monitoring according to U.S. EPA Methods 300.0, 314 and 218.6.
Monitoring and maintaining water purity are important to the power and electronics industries. In the both of these industries, impurities must be minimized and monitored to prevent corrosion or scaling, and degradation in demineralization processes. Learn about the analysis of ppb concentrations of ionic contaminants in high purity water using two easy methods: a direct large volume injection and concentration of a large volume injection, using electrolytically generated hydroxide eluents on a Reagent-Free™ Ion Chromatography system (RFIC™).
The slickwater stimulation of unconventional gas and oil shale plays creates flowback water with a composition that is unique to particular shale formations. Characteristically, these fluids contain high concentrations of salts (e.g., chloride, bromide) which are routinely determined using ion chromatography. This analysis typically requires sample preparation, including manual dilution, which can significantly increase the cost of analysis. Results presented will show highly reproducible determination of anions and cations from Marcellus Shale flowback water using inline conductivity to identify high salt samples and then automatically diluting them prior to injection, saving time and column life.
Wastewater is produced by multiple sources, including chemical manufacturing, power generation, petroleum product extraction, and private residences. Specific industries can use knowledge of around the analytes present in wastewater to make decisions on reuse, treatment, or whether disposal is the most cost effective option. Prior to any discharge into ground or surface waters, the level of specific analytes must be determined to ensure that they do not exceed regulated limits. If these limits are being exceeded, treatment will be required. Ion Chromatography (IC) is the primary technique used for measuring the concentration of ions in wastewater and numerous methods have been developed that meet regulatory requirements. Learn about IC methods that enable accurate, consistent, and rapid measurement of both anions, such as chloride, sulfate, and bromate, and cations, such as sodium and magnesium.
In the past, measuring the total amount of an element was sufficient. Unfortunately, the effects of an element extend far beyond its absolute amount. Different forms of an element can exhibit very different physicochemical properties, including varying toxicities. The process of separation and quantification of different chemical forms of an element, more specifically termed speciation analysis, can be utilized to determine an element’s various chemical forms. The number of environmental applications of elemental speciation analysis has increased significantly. For example, both the United States EPA and the European Union have specified maximum admissible chromium concentrations in their respective drinking water directives and are evaluating the inclusion of hexavalent chromium in certain legislation. Learn about the latest developments in chromatography technology for speciation analysis that offer data for a wide variety of applications, including chromium in drinking water and both arsenic and sulfur in environmental waters.
More from Chromatography & Mass Spectrometry Solutions (20)
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.
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.
A brief information about the SCOP protein database used in bioinformatics.
The Structural Classification of Proteins (SCOP) database is a comprehensive and authoritative resource for the structural and evolutionary relationships of proteins. It provides a detailed and curated classification of protein structures, grouping them into families, superfamilies, and folds based on their structural and sequence similarities.
Introduction:
RNA interference (RNAi) or Post-Transcriptional Gene Silencing (PTGS) is an important biological process for modulating eukaryotic gene expression.
It is highly conserved process of posttranscriptional gene silencing by which double stranded RNA (dsRNA) causes sequence-specific degradation of mRNA sequences.
dsRNA-induced gene silencing (RNAi) is reported in a wide range of eukaryotes ranging from worms, insects, mammals and plants.
This process mediates resistance to both endogenous parasitic and exogenous pathogenic nucleic acids, and regulates the expression of protein-coding genes.
What are small ncRNAs?
micro RNA (miRNA)
short interfering RNA (siRNA)
Properties of small non-coding RNA:
Involved in silencing mRNA transcripts.
Called “small” because they are usually only about 21-24 nucleotides long.
Synthesized by first cutting up longer precursor sequences (like the 61nt one that Lee discovered).
Silence an mRNA by base pairing with some sequence on the mRNA.
Discovery of siRNA?
The first small RNA:
In 1993 Rosalind Lee (Victor Ambros lab) was studying a non- coding gene in C. elegans, lin-4, that was involved in silencing of another gene, lin-14, at the appropriate time in the
development of the worm C. elegans.
Two small transcripts of lin-4 (22nt and 61nt) were found to be complementary to a sequence in the 3' UTR of lin-14.
Because lin-4 encoded no protein, she deduced that it must be these transcripts that are causing the silencing by RNA-RNA interactions.
Types of RNAi ( non coding RNA)
MiRNA
Length (23-25 nt)
Trans acting
Binds with target MRNA in mismatch
Translation inhibition
Si RNA
Length 21 nt.
Cis acting
Bind with target Mrna in perfect complementary sequence
Piwi-RNA
Length ; 25 to 36 nt.
Expressed in Germ Cells
Regulates trnasposomes activity
MECHANISM OF RNAI:
First the double-stranded RNA teams up with a protein complex named Dicer, which cuts the long RNA into short pieces.
Then another protein complex called RISC (RNA-induced silencing complex) discards one of the two RNA strands.
The RISC-docked, single-stranded RNA then pairs with the homologous mRNA and destroys it.
THE RISC COMPLEX:
RISC is large(>500kD) RNA multi- protein Binding complex which triggers MRNA degradation in response to MRNA
Unwinding of double stranded Si RNA by ATP independent Helicase
Active component of RISC is Ago proteins( ENDONUCLEASE) which cleave target MRNA.
DICER: endonuclease (RNase Family III)
Argonaute: Central Component of the RNA-Induced Silencing Complex (RISC)
One strand of the dsRNA produced by Dicer is retained in the RISC complex in association with Argonaute
ARGONAUTE PROTEIN :
1.PAZ(PIWI/Argonaute/ Zwille)- Recognition of target MRNA
2.PIWI (p-element induced wimpy Testis)- breaks Phosphodiester bond of mRNA.)RNAse H activity.
MiRNA:
The Double-stranded RNAs are naturally produced in eukaryotic cells during development, and they have a key role in regulating gene expression .
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.
This pdf is about the Schizophrenia.
For more details visit on YouTube; @SELF-EXPLANATORY;
https://www.youtube.com/channel/UCAiarMZDNhe1A3Rnpr_WkzA/videos
Thanks...!
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.
Observation of Io’s Resurfacing via Plume Deposition Using Ground-based Adapt...
Chromatography: Meeting the Challenges of EU regulations with up-to-date Confirmatory Solutions
1. Meeting the challenges of EU regulations with up-to-date confirmatory solutions
Lunch Seminar at the 34th International Symposium on Halogenated Persistent Organic Pollutants (Dioxin 2014)
2. Validation of a triple quadrupole GC-MS/MS technology for detection, quantification and confirmation of low level dioxins in feed and food samples
Cristian Cojocariu, PhD
ThermoFisher Scientific, Runcorn, UK
3. 3
Overview
•Thermo Scientific™ TSQ 8000™ Evo triple quadrupole GC-MS was used to detect and confirm low level of PCDD/Fs in sample extracts, taking into account the EU Commission Regulation 589/2014 and the new Regulation No. 709/2014
•A thorough validation of the TSQ 8000 Evo GC-MS/MS for dioxin confirmation was performed.
•Instrument sensitivity, linearity, chromatography, LOD/LOQs and precision of measurements were assessed.
•Data acquired using the GC-MS/MS was compared with the GC-HRMS data acquired for the same samples and measurements uncertainties were assessed.
5. 5
TSQ 8000 Evo GC-MS System
•State of the art triple quadrupole GC-MS system introduced at ASMS 2014
•Fast collision cell instrument with enhanced velocity optics with EvoCell technology to provide high SRM transition speeds, precision and sensitivity
•ExtractaBrite™ ion source is heated throughout ensuring high matrix tolerance
•Ion source fully removable, hot, under vacuum when cleaning is necessary or swapping with a spare; no vent to clean your instrument
6. 6
GC & MS Conditions
Thermo Scientific™ TRACE™ 1310 GC Parameters
Column
TG-5 SIL MS, 60 m x 0.25 x 0.25
Injection Volume (mL):
2
Liner
SSL single taper 4mm ID 78.5mm
Inlet (°C):
260
Inlet Module and Mode:
splitless
Carrier Gas, (mL/min):
He, 1.2
Oven Temperature Program time (min):
33
TSQ 8000 Evo Mass Spectrometer Parameters
Transfer line (°C):
280
Ionization type:
EI
Ion source(°C):
300
Electron energy (eV):
40
Acquisition Mode:
SRM
Q1 Peak Width (AMU):
0.7
Q3 Peak Width (AMU):
0.7
GC
MS
7. 7
Samples
•Wellington Lab standards used in the experiments described below: EPA1613 calibration set
TF-TCDD-MXD
Compound
Concentration (fg/μL)
1368-TCDD
10
1379-TCDD
25
1378-TCDD
100
1478-TCDD
250
1234-TCDD
500
2378-TCDD
1000
8. 8
Samples
•Matrix samples (previously analysed on a GC-HRMS instrument) provided by EU-RL, Freiburg
•Samples chosen were naturally contaminated with low level of PCDD/Fs.
•Used to assess and validate the LOQs in matrix samples as well as to check precision of total dioxin content at low level.
•Extraction and clean-up was carried out in accordance with the existing methods for food and feed either automatically (PowerPrep™ SPE) or partly manual/partly automated (GPC, multi-layer silica, Florisil®, carbon).
Mixed animal fat
Fish meal
Egg fat 11
Egg fat 2
Weighted sample:
10.0 g fat
60.2 g sample (= 10.0 g fat)
0.52 g fat
0.51 g fat
Lipid content [%]:
n/a
16.6
n/a
n/a
Moisture content [%]:
n/a
5.3
n/a
n/a
Final volume:
40 μl
40 μl
10 μl
10 μl
13C Internal standard
13C Internal standard
13C Internal standard
13C Internal standard
2378 TCDF
50
50
10
10
12378 PCDF
50
50
10
10
23478-PCDF
200
200
40
40
123478 HxCDF
100
100
20
20
123678 HxCDF
100
100
20
20
234678 HxCDF
50
50
10
10
123789 HxCDF
50
50
10
10
1234678 HpCDF
100
100
20
20
1234789 HpCDF
50
50
10
10
OCDF
100
100
20
20
2378 TCDD
50
50
10
10
12378 PCDD
100
100
20
20
123478 HxCDD
100
100
20
20
123678 HxCDD
200
200
40
40
123789 HxCDD
50
50
10
10
1234678 HpCDD
200
200
40
40
OCDD
600
600
120
120
13C Recovery standard
13C Recovery standard
13C Recovery standard
13C Recovery standard
1234-TCDD
50
50
10
10
9. 9
Data Acquisition and Data Processing
•Data were acquired using timed-Selected Reaction Monitoring (timed-SRM).
•A minimum of 12 points/chromatographic peak were acquired.
•Data processing was performed with Thermo Scientific™ TargetQuan 3.1 software.
10. 10
Linearity of Response
•Linearity assessed by determining the average RF %RSD values from a six point calibration curve measured at the beginning and at the end of the sample batch.
•Values represent duplicate measurements of each calibration point, measured at the beginning and end of a batch.
Compound
Concentration range (pg/μL)
Average RF
stdev
RF %RSD
2378-TCDF
0.1 - 40
1.0
0.04
3.7
2378-TCDD
0.1 - 40
1.4
0.02
1.4
12378-PeCDF
0.5 - 200
1.0
0.01
0.9
23478-PeCDF
0.5 - 200
1.0
0.02
1.8
12378-PeCDD
0.5 - 200
1.2
0.03
2.5
123478-HxCDF
0.5 - 200
1.0
0.01
0.8
123678-HxCDF
0.5 - 200
1.0
0.01
1.3
234678-HxCDF
0.5 - 200
1.0
0.01
1.3
123478-HxCDD
0.5 - 200
0.9
0.01
0.7
123678-HxCDD
0.5 - 200
1.1
0.01
1.3
123789-HxCDD
0.5 - 200
1.0
0.01
0.7
123789-HxCDF
0.5 - 200
1.0
0.05
4.5
1234678-HpCDF
0.5 - 200
1.1
0.01
0.9
1234678-HpCDD
0.5 - 200
1.1
0.01
1.0
1234789-HpCDF
0.5 - 200
1.1
0.02
1.4
OCDD
1.0 - 400
1.5
0.02
1.6
OCDF
1.0 - 400
1.1
0.02
1.4
11. 11 Determination of Limit of Quantification
•LOQ calculated from CSL x5 and CSL x10 dilution and taking into account the ion ratio, response factors and precision limits.
•LOQ for each native compound was calculated taking into account the student’s-t critical values for the corresponding degrees of freedom (99% confidence).
Compound
pg/μL
2378-TCDF
0.01
2378-TCDD
0.01
12378-PeCDF
0.02
23478-PeCDF
0.02
12378-PeCDD
0.02
123478-HxCDF
0.04
123678-HxCDF
0.04
234678-HxCDF
0.03
123478-HxCDD
0.06
123678-HxCDD
0.03
123789-HxCDD
0.04
123789-HxCDF
0.04
1234678-HpCDF
0.02
1234678-HpCDD
0.05
1234789-HpCDF
0.02
OCDD
0.05
OCDF
0.03
12. 12
Sensitivity test: stepped standard
• Overlayed SRM chromatograms (quan ion) of six TCDD congeners in the stepped
standard.
• Concentrations represents ‘on column’ amount.
RT: 13.37 - 14.94 SM: 3B
13.4 13.5 13.6 13.7 13.8 13.9 14.0 14.1 14.2 14.3 14.4 14.5 14.6 14.7 14.8 14.9
Time (min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
14.78
14.57
14.30
14.15
13.65
13.52 14.86 13.53 13.76 14.38 14.41 14.67
14.56
NL: 8.47E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_11
NL: 8.33E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_03
NL: 8.49E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_05
NL: 8.25E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_06
NL: 8.35E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_07
NL: 8.38E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_08
NL: 8.53E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_09
NL: 8.48E4
TIC F: + c EI SRM ms2
321.890@cid20.00
[258.925-258.935] MS
19May2014_10
1368-TCDD
10 fg
IR % = 9
1379-TCDD
25 fg
IR % = 6
1378-TCDD
100 fg
IR % = 7
1478-TCDD
250 fg
IR % = 6
2378-TCDD
1000 fg
IR % = 4
1234-TCDD
500 fg
IR % = 11
Inj. No. Concentration
10 fg 25 fg 100 fg 250 fg 500 fg 1000 fg
1 3129 7011 25940 60219 87635 239216
2 3045 6209 25998 59108 85789 240162
3 3047 7055 27425 58262 87578 237274
4 2637 7440 25734 59335 87079 233655
5 2678 6376 27805 58583 83897 234470
6 2964 6513 27097 58902 85373 238554
7 2828 6931 26347 59936 86844 242740
8 2699 6579 25033 55519 79471 232038
mean 2878.4 6764.3 26422.4 58733.0 85458.3 237263.6
STDEV 192.5 411.7 940.7 1452.1 2730.3 3625.3
% RSD 6.7 6.1 3.6 2.5 3.2 1.5
14. 14 Quantification of Dioxins in the Sample Extracts
•The egg, animal fat and fish meal samples were analyzed for their dioxin content.
•The calculated concentration of each individual dioxin congener (pg TEQ/g fat or ng/kg %dw) was compared with the values obtained from the GC-HRMS.
18. 18
Ion Ratio Stability: IR Egg Sample vs. Theoretical IR
19. 19 Ion Ratio Stability: IR Egg Sample vs. IR CS3
20. 20
Precision of Measurements: Sample Extracts
•Obtaining valid estimates of PCDD/Fs concentration in sample extracts is critical.
•Precision measurement of the total dioxin content (as WHO TEQ pg/g or ng/kg) for a sequence of n=13 repeat injections of the mixed animal fat and the fish meal samples
21. 21 Fish Meal: Precision of Total Dioxin Content (n=13)
22. 22
Mixed Animal Fat: Precision of Total Dioxin Content (n=13)
23. 23
Comparison with GC-HRMS
Total dioxin content of sample extracts
•Average values of replicate injections (n) with corresponding standard deviations (in brackets) are given.
Sample type
WHO-PCDD/F-TEQ-ub
GC-HRMS
GC-MS/MS
Deviation %
egg (n=2)
3.39 pg/g
3.27 (0.03)
-3.5
fish meal (n=13)
0.26 ng/kg % dw
0.25 (0.01)
-2.2
mixed animal fat (n=13)
0.83 pg/g
0.85 (0.04)
2.8
24. 24
Conclusions
•Excellent selectivity and sensitivity was achieved (ex: 28 fg 2378-TCDD absolute amount on column)
•Precision measurements of the total dioxin content (WHO-PCDD/F-TEQ-ub) were obtained for two low level contaminated samples (fish meal and mixed animal fat) with %RSD values <6% (n=13).
•Deviation of the total dioxin content (WHO-PCDD/F-TEQ-ub) from the GC-HRMS data was analyzed within the ±20% for all the samples.
•The data shows excellent agreement between the results obtained using the TSQ 8000 Evo GC-MS/MS and those obtained using GC-HRMS.
•TSQ 8000 Evo triple quadrupole system is a sensitive and robust system suitable for the quantification and confirmation of low level dioxins and furans in food and feed matrices.
26. 26 Thank You for Your Attention! Stay connected with us Twitter @ChromSolutions Chromatography Solutions Blog http://chromblog.thermoscientific.com/blog YouTube http://www.youtube.com/ChromSolutions Facebook http://www.facebook.com/ChromatographySolutions Pinterest http://pinterest.com/chromsolutions/
27. Economic POPs
Dave Hope, Patrick Pond, Wasana Mudalige, Jose del Pozo, Matt Wright
Pacific Rim Laboratories Inc.
Presented at Thermo Scientific Vendor Seminar
Madrid, Spain September 2,2014
28. Outline
•
Cost of Analysis
•
Saving time on extraction - Accelerated Solvent Extraction (ASE)
•
Saving time and money on clean-up - Cape Technologies Clean-up Kits
•
Is GC-MS/MS technology ready for POPs – Thermo Scientific™ TSQ™ 8000 system
29. Economic Costs – POPs Lab
•
Laboratory
–
$1-3M or higher if budget allows
•
Instrument
–
$150-400k up to $250-600k depending on options
•
Staffing (2-10)
–
$20-50 per hour ($40-100k per annum)
•
Soft costs
–
Chemicals 7-10% revenue
–
Consumables 5-10% revenue
–
Service contracts/R&M 5-7% revenue or 5-10% instrument cost
–
Staff Training 6 weeks to 6 months or $5-35k
30. Cost of Analysis
•
Sample Extraction (batch of 10 samples)
–
Water: liquid/liquid sep funnel 6-8 h
–
Soil/tissue: soxhlet 6-8 h
–
Tissue: acid digestion 12 h
–
@ $20 per hour with 10 sample batch $16-24
–
@ $20 per hour with 6 sample batch $25-40
–
@ $20 per hour with 2 sample batch $50-75
31. Sample clean-up
•
Clean-up steps (4-8 h each)
–
Acid or base washes
–
Acid/base silica gel
–
Basic Alumina
–
Florisil (separate dioxins and PCBs)
–
Carbon
•
Soft costs
–
Preparing reagents
–
Cleaning reusable glassware – 2 h per day
–
Re-analyzing cross contaminated samples
32. Simplified Clean-up for Food and Environmental Sample
•
Cape Technologies tandem acid silica gel / carbon columns
–
Originally designed as clean-up kit for EPA Method 4025 (Screening for PCDD/F by Immunoassay)
–
quick and cheap – 4-6 h to complete 12 samples, <$20/sample disposable columns, $500 hardware
–
Columns are disposable, therefore reduces PCB carryover from improper washing of reusable columns (not to mention the labor savings)
–
Separates dioxins from PCBs
–
Separates dl PCBs from interfering PCBs with high LOC
–
Yang et al (MOE Ontario) developed method to separate PCB, PBDE and PCDD/F (Dioxin 2010)
33. Cape Technologies Clean-up Kit
•
Glass column, 15 mm x 27 cm, loaded with 5 g acid (30%) silica gel (63-200 μm)
•
25 mm column available with 14 or 28 g acid (50%) silica (32-63 μm)
•
Each column individually sealed, wrapped in boxes of 12
•
Carbon soxhlet extracted with Toluene prior to packing in Teflon column (one end flat and the other end bevelled for easy identification of flow direction)
•
150 mg of 2% carbon in FEP Teflon
34. Columning Procedure
•
Pre-rinse carbon column
–
10 mL toluene
–
10 mL DCM
–
30 mL hexane
•
Attached carbon column to acid silica gel – bevelled side down
•
Load sample in 1-2 mL hexane
•
Elute 30 mL hexane (F1) – pressurize to 10 psi (1-2 mL/min)
•
Remove carbon and attach to empty glass column
•
Elute 6 mL 1:1 toluene/hexane (F2)
•
Reverse carbon column flow
•
Elute 30 mL toluene (F3)
35. F3 – PCDD/F
•
All 17 congeners found in F3
•
Spike recoveries for TeCDD/F- HpCDD/F were 93-107% with RSD<12%
•
Recovery of OCDD was 85% and OCDF 49%
•
There may be some loss of non-2,3,7,8 congeners (especially TeCDD/F)
•
Cut point between F2/F3 tight for TeCDD/F (F2 max volume 6 mL of 50:50 toluene/hexane)
36. Accelerated Solvent Extraction (ASE)
•
Has been widely used for soils and tissues in conventional analyses (ppm/ppb)
•
Cells and lines subject to trace contamination and carry over at ultra-trace levels
•
Recently given an Thermo Scientific™ Dionex™ ASE™ 350 Accelerated Solvent Extractor to play with complete with 100 mL Thermo Scientific™ Dionium™ cells
•
Thermo Fisher Scientific has application notes for tissue samples using max 1 g lipid
•
PRL methodology requires 5-10 g lipid for lowest DLs
•
Initial problems with packing cells – critical not to
–
over pack them – SOLVENT LEAKAGE WARNING
–
under pack them – VAPOUR PRESSURE WARNING
•
Instrument lines and cells required thorough cleaning after installation
37. ASE 350 System
Extraction Conditions
Extraction Solvent: Hexane/Acetone 3:1
Temperature: 100 °C
Pressure: 1600 psi
Heat Time: 5 min
Static Time: 5 min
Flush Volume: 70%
Purge Time: 120 s
Static Cycles: 3
Total Prep Time: 15 min per sample
Total Extraction Time: 25 min per sample
38. Butter (n=5)
Units: ng/kg (pg/g)
Control
Average
Spike
Recovery
RSD
2378-TCDD
<0.03
<0.03
20
91%
15%
12378-PeCDD
<0.033
<0.033
100
94%
5%
123478-HxCDD
0.15
0.20
100
82%
14%
123678-HxCDD
0.56
0.60
100
87%
8%
123789-HxCDD
0.18
0.25
100
90%
3%
1234678-HpCDD
1.21
1.69
100
96%
7%
OCDD
0.88
1.83
200
95%
2%
2378-TCDF
<0.03
<0.03
100
94%
11%
12378-PeCDF
<0.039
0.07
100
92%
5%
23478-PeCDF
<0.039
<0.039
100
90%
8%
123478-HxCDF
0.16
0.24
100
82%
14%
123678-HxCDF
0.12
0.12
100
86%
9%
123789-HxCDF
<0.056
<0.056
100
93%
5%
234678-HxCDF
0.11
0.20
100
80%
16%
1234678-HpCDF
<0.052
<0.052
100
88%
12%
1234789-HpCDF
<0.085
<0.085
100
87%
9%
OCDF
<0.13
0.20
200
66%
6%
Use 6.25 g of butter (80% lipid) mixed with 10 g diatomaceous earth
Add internal standards
Pack 100 mL Dionium cell with
•
30 mm cellulose filter
•
10 g Dionex ASE Prep CR Na+ form (sulphonated divinyl benzene/styrene copolymer)
•
Add sample mix
•
Top with diatomaceous earth to 10 mm from top of cell
Cape Technologies column clean-up
41. Can economy model TSQ 8000 GC/MS run PCDD/F
•
Benchtop instrument
•
More affordable
•
Increased uptime
•
Easier maintenance
•
Lower electrical usage
42. So easy anyone can learn???
•
It helps if you know how to type!
•
Monitor M-COCl
–
No chlorinated diphenylether interference
•
EPA 1613b calibration, with CS- Lo and 0.2 x CS-Lo
45. Data Comparison ASE – Cape Tech – TSQ 8000 MS
•
Ten vials of CARP-2 (ground whole carp reference material) from NRC Canada
•
Reference concentrations for PCDD/F and select PCBs (several congeners in excess of 100 ug/kg)
•
Entire contents of vial (approx 10 g) extracted using ASE 350
•
Cape Technologies tandem acid silica gel / carbon clean-up
•
Analysis by DFS HRMS System
•
Analysis by TSQ 8000 Triple Quadrupole GC-MS
48. Conclusions
•
Cape Technologies provides a simple, inexpensive clean-up for dioxins and PCBs
•
ASE can be made clean and effective for food samples at ppq levels
•
TSQ 8000 GC-MS system has the sensitivity and specificity to analyze PCDD/F from food extracts.