This document discusses the principles and instrumentation of high performance thin layer chromatography coupled with mass spectrometry (HPTLC-MS). HPTLC-MS combines the separation capabilities of HPTLC with the identification abilities of mass spectrometry. It works by separating compounds via HPTLC and then using an interface to extract zones of interest from the HPTLC plate and transfer them to a mass spectrometer for analysis. This allows for structural confirmation and elucidation of targeted analytes. Some advantages of HPTLC-MS are that it is cost-effective, allows identification of unknown substances, and is useful for applications like drug analysis, metabolism studies, and characterization of impurities.
The versatile instrument is used to isolate unknown compounds from a HPTLC/TLC plate and transfer them into a mass spectrometer for identification or structure elucidation.
Hyphenated technique is a combination or coupling of two analytical techniques with the help of proper interface.
In this presentation Hyphenated techniques-LC-MS/MS, GC-MS/MS, HPTLC-MS has been discussed
The aim of the coupling is to obtain an information-rich detection for both identification and quantification compared to that with a single analytical technique.
It is instrumental analytical technique. it is one of the major type of chromatography technique. its basic principle is adsorption. it has many applications in various fields
The versatile instrument is used to isolate unknown compounds from a HPTLC/TLC plate and transfer them into a mass spectrometer for identification or structure elucidation.
Hyphenated technique is a combination or coupling of two analytical techniques with the help of proper interface.
In this presentation Hyphenated techniques-LC-MS/MS, GC-MS/MS, HPTLC-MS has been discussed
The aim of the coupling is to obtain an information-rich detection for both identification and quantification compared to that with a single analytical technique.
It is instrumental analytical technique. it is one of the major type of chromatography technique. its basic principle is adsorption. it has many applications in various fields
Hyphenated Techniques - coupling of a separation technique and an on-line spectroscopic detection technology.
Advantages of hyphenated techniques;
1. Fast and accurate analysis.
2. Higher degree of automation.
3. Higher sample throughput.
4. Better reproducibility.
5. Reduction of contamination due to its closed system.
6. Separation and quantification achieved at same time.
The objective of any chemical analytical measurement is to get consistent, reliable and accurate data.
Proper functioning and performance of analytical instruments and computer systems plays a major role in achieving this goal.
Therefore, analytical instrument qualification (AIQ) and calibration should be part of any good analytical practice.
High Performance Thin Layer Chromatography (HPTLC) instrumentationMadhuraNewrekar
HPTLC is an advancement of TLC. It is a high performance liquid chromatography with automation compared to Thin Layer Chromatography(TLC).Speed, Efficiency and Accuracy are important advantages. Evaluation time is less due to updated automation in instrumentation.
Steps involved in HPTLC and the materials and instruments required in those steps are described in brief.
CALIBRATION OF HPLC
Pressure Test.
Drift and Noise
Column oven and sample cooler
Pump by flow rate accuracy measurement.
Pump by gradient flow measurement.
UV-Vis / PDA detector by reference energy check.
The hyphenated technique is a combination or coupling of two analytical techniques with the help of a proper interface.
The aim of the coupling is to obtain an information-rich detection for both identification and quantification compared to that with a single analytical technique.
Hyphenated Techniques - coupling of a separation technique and an on-line spectroscopic detection technology.
Advantages of hyphenated techniques;
1. Fast and accurate analysis.
2. Higher degree of automation.
3. Higher sample throughput.
4. Better reproducibility.
5. Reduction of contamination due to its closed system.
6. Separation and quantification achieved at same time.
The objective of any chemical analytical measurement is to get consistent, reliable and accurate data.
Proper functioning and performance of analytical instruments and computer systems plays a major role in achieving this goal.
Therefore, analytical instrument qualification (AIQ) and calibration should be part of any good analytical practice.
High Performance Thin Layer Chromatography (HPTLC) instrumentationMadhuraNewrekar
HPTLC is an advancement of TLC. It is a high performance liquid chromatography with automation compared to Thin Layer Chromatography(TLC).Speed, Efficiency and Accuracy are important advantages. Evaluation time is less due to updated automation in instrumentation.
Steps involved in HPTLC and the materials and instruments required in those steps are described in brief.
CALIBRATION OF HPLC
Pressure Test.
Drift and Noise
Column oven and sample cooler
Pump by flow rate accuracy measurement.
Pump by gradient flow measurement.
UV-Vis / PDA detector by reference energy check.
The hyphenated technique is a combination or coupling of two analytical techniques with the help of a proper interface.
The aim of the coupling is to obtain an information-rich detection for both identification and quantification compared to that with a single analytical technique.
Levelwise PageRank with Loop-Based Dead End Handling Strategy : SHORT REPORT ...Subhajit Sahu
Abstract — Levelwise PageRank is an alternative method of PageRank computation which decomposes the input graph into a directed acyclic block-graph of strongly connected components, and processes them in topological order, one level at a time. This enables calculation for ranks in a distributed fashion without per-iteration communication, unlike the standard method where all vertices are processed in each iteration. It however comes with a precondition of the absence of dead ends in the input graph. Here, the native non-distributed performance of Levelwise PageRank was compared against Monolithic PageRank on a CPU as well as a GPU. To ensure a fair comparison, Monolithic PageRank was also performed on a graph where vertices were split by components. Results indicate that Levelwise PageRank is about as fast as Monolithic PageRank on the CPU, but quite a bit slower on the GPU. Slowdown on the GPU is likely caused by a large submission of small workloads, and expected to be non-issue when the computation is performed on massive graphs.
Opendatabay - Open Data Marketplace.pptxOpendatabay
Opendatabay.com unlocks the power of data for everyone. Open Data Marketplace fosters a collaborative hub for data enthusiasts to explore, share, and contribute to a vast collection of datasets.
First ever open hub for data enthusiasts to collaborate and innovate. A platform to explore, share, and contribute to a vast collection of datasets. Through robust quality control and innovative technologies like blockchain verification, opendatabay ensures the authenticity and reliability of datasets, empowering users to make data-driven decisions with confidence. Leverage cutting-edge AI technologies to enhance the data exploration, analysis, and discovery experience.
From intelligent search and recommendations to automated data productisation and quotation, Opendatabay AI-driven features streamline the data workflow. Finding the data you need shouldn't be a complex. Opendatabay simplifies the data acquisition process with an intuitive interface and robust search tools. Effortlessly explore, discover, and access the data you need, allowing you to focus on extracting valuable insights. Opendatabay breaks new ground with a dedicated, AI-generated, synthetic datasets.
Leverage these privacy-preserving datasets for training and testing AI models without compromising sensitive information. Opendatabay prioritizes transparency by providing detailed metadata, provenance information, and usage guidelines for each dataset, ensuring users have a comprehensive understanding of the data they're working with. By leveraging a powerful combination of distributed ledger technology and rigorous third-party audits Opendatabay ensures the authenticity and reliability of every dataset. Security is at the core of Opendatabay. Marketplace implements stringent security measures, including encryption, access controls, and regular vulnerability assessments, to safeguard your data and protect your privacy.
Adjusting primitives for graph : SHORT REPORT / NOTESSubhajit Sahu
Graph algorithms, like PageRank Compressed Sparse Row (CSR) is an adjacency-list based graph representation that is
Multiply with different modes (map)
1. Performance of sequential execution based vs OpenMP based vector multiply.
2. Comparing various launch configs for CUDA based vector multiply.
Sum with different storage types (reduce)
1. Performance of vector element sum using float vs bfloat16 as the storage type.
Sum with different modes (reduce)
1. Performance of sequential execution based vs OpenMP based vector element sum.
2. Performance of memcpy vs in-place based CUDA based vector element sum.
3. Comparing various launch configs for CUDA based vector element sum (memcpy).
4. Comparing various launch configs for CUDA based vector element sum (in-place).
Sum with in-place strategies of CUDA mode (reduce)
1. Comparing various launch configs for CUDA based vector element sum (in-place).
Techniques to optimize the pagerank algorithm usually fall in two categories. One is to try reducing the work per iteration, and the other is to try reducing the number of iterations. These goals are often at odds with one another. Skipping computation on vertices which have already converged has the potential to save iteration time. Skipping in-identical vertices, with the same in-links, helps reduce duplicate computations and thus could help reduce iteration time. Road networks often have chains which can be short-circuited before pagerank computation to improve performance. Final ranks of chain nodes can be easily calculated. This could reduce both the iteration time, and the number of iterations. If a graph has no dangling nodes, pagerank of each strongly connected component can be computed in topological order. This could help reduce the iteration time, no. of iterations, and also enable multi-iteration concurrency in pagerank computation. The combination of all of the above methods is the STICD algorithm. [sticd] For dynamic graphs, unchanged components whose ranks are unaffected can be skipped altogether.
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Empowering the Data Analytics Ecosystem: A Laser Focus on Value
The data analytics ecosystem thrives when every component functions at its peak, unlocking the true potential of data. Here's a laser focus on key areas for an empowered ecosystem:
1. Democratize Access, Not Data:
Granular Access Controls: Provide users with self-service tools tailored to their specific needs, preventing data overload and misuse.
Data Catalogs: Implement robust data catalogs for easy discovery and understanding of available data sources.
2. Foster Collaboration with Clear Roles:
Data Mesh Architecture: Break down data silos by creating a distributed data ownership model with clear ownership and responsibilities.
Collaborative Workspaces: Utilize interactive platforms where data scientists, analysts, and domain experts can work seamlessly together.
3. Leverage Advanced Analytics Strategically:
AI-powered Automation: Automate repetitive tasks like data cleaning and feature engineering, freeing up data talent for higher-level analysis.
Right-Tool Selection: Strategically choose the most effective advanced analytics techniques (e.g., AI, ML) based on specific business problems.
4. Prioritize Data Quality with Automation:
Automated Data Validation: Implement automated data quality checks to identify and rectify errors at the source, minimizing downstream issues.
Data Lineage Tracking: Track the flow of data throughout the ecosystem, ensuring transparency and facilitating root cause analysis for errors.
5. Cultivate a Data-Driven Mindset:
Metrics-Driven Performance Management: Align KPIs and performance metrics with data-driven insights to ensure actionable decision making.
Data Storytelling Workshops: Equip stakeholders with the skills to translate complex data findings into compelling narratives that drive action.
Benefits of a Precise Ecosystem:
Sharpened Focus: Precise access and clear roles ensure everyone works with the most relevant data, maximizing efficiency.
Actionable Insights: Strategic analytics and automated quality checks lead to more reliable and actionable data insights.
Continuous Improvement: Data-driven performance management fosters a culture of learning and continuous improvement.
Sustainable Growth: Empowered by data, organizations can make informed decisions to drive sustainable growth and innovation.
By focusing on these precise actions, organizations can create an empowered data analytics ecosystem that delivers real value by driving data-driven decisions and maximizing the return on their data investment.
2. Principle
• HPTLC based on simple principle which is separation of compound from
sample by adsorption phenomena.
• The basic principle of mass spectrometry (MS) is to generate ions from
either inorganic or organic compounds by any suitable method, to
separate these ions by their mass-to-charge ratio (m/z) and to detect
them qualitatively and quantitatively by their respective m/z and
abundance
• It is versatile tech. for separation as well as identification of pharmaceutical and
phytochemical.
• Traditionally the separation was carried out TLC separation and separation was
removed to study/identify in mass spectroscopy.
• The use of HPTLC and combination with high resolution TOF mass spectroscopy
for the detection, identify and imaging resulting in increase in analytical
importance.
3.
4. Instrumentation
*For this follow HPTLC and mass spectroscopy instrumentation.
HPTLC:
• Sample Preparation
• Selection of Chromatographiclayers
• Plates
• Pre washing
• Conditioning
• Sample Application
• Pre conditioning
• Mobile Phase
• Chromatographic Development
• Detection of spot
• Scanning and Documentation
(*SEE HPTLC NOTE)
5. Interfaces:
High performance thin layer chromatography (Camag, Muttanz, Switzerland) consisted of an
auto sample applicator Linomat V connected to a nitrogen cylinder, TLC scanner attached to a
PC running win-CATS software (version 1.4.4), TLC Visualizer, and Camag twin-trough chambers
were used in analysis. HPTLC-MS detailed examination was carried out by TLC-MS interface
using acetonitrile as eluting agent at a flow rate of 1 ml/min. It remove/take out circular zones
in the form of bands from the developed HPTLC plate. The eluted material was transferred
automatically to single-quadrupole mass spectrometer, and mass spectra was recorded.
Surveys have shown that not all samples may be processed by HPTLC-MS or HPTLC-DAD or
HPTLC-MALDI or low delectability of the compounds or impurities in the UV range, a heavy
matrix load or a deficiency of MS compatible solvents. On the other hand HPTLC is another
very fast and suitable method to separate samples. In the past unknown substances were
scraped off from the TLC/HPTLC plate, eluted into a tube with solvent and transferred into the
MS. Now a very suitable and universal TLC-MS Interface is available which can semi-
automatically extract zones of interest and direct them online into any brand of HPLC-MS
system. The interface is fast and simply connected (by two fittings) to any LC-coupled mass
spectrometer without adjustments or mass spectrometer modifications. Questioned materials
are directly extracted from a TLC/HPTLC plate and sensitive mass spectrometric signals are
obtained within a minute per substance zone. The interface extracts the complete material
zone with its depth profile and thus allows detections comparable to HPLC down to the
pg/zone range. The interface has been demonstrate to be one of the most reliable and
versatile interfaces for TLC/HPTLC-MS coupling.
6. Mass spectroscopy:
Ion source
High vacuum system
Mass analyzer
Ion collector data system
(*SEE GC-MS OR MS NOTE)
Advantage of HPTLC-MS
It is cost effective because the chromatography run in decoupled with the detection
step.
7. Advantage
HPTLC-MS is a strong additional detection possibility and allows the structural
confirmation of targeted analytes. It also allows to do structure elucidation by coupling
HPTLC to high-resolution MS.
8. CONCLUSION:
1. This above short report a simple hptlc-ms method for the the routine analysis of
pharmaceutical product/formulation.
2.Its play important role in the study of the drug metabolism, discovery of new drug
candidate and the analysis, identification and characterization of impurities and degradent in
drug substants.
3. With regard to the outcome of this study and recommendations for plate handling, special
plate forms are rational.
4.The hptlc-ms interface is versatile building block of multidimensional liquid
chromatographic system.
5. Lc-ms have proved to be an extremely sensitive and specific technique for the analysis of
pharmaceutical product.
Application:
1. The liquid chromatography–mass spectrometry study of degraded products gave the idea
about the fragmentation patterns of degraded products. The developed method can be used
for routine analysis of terizidone and its formulations.
2. Degradation product of Empagliflozin in alkaline condition was carried out and its
degradation product is successfully separated and isolated by HPTLC method. degradation
product was identified by using MS-MS technique.
