News from LabRulezLCMS Library - Week 38, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 16th September 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!

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This week we bring to you applications, technical notes, posters, and other documents by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, Waters Corporation, Metrohm, and Galochrom!

1. Galochrom: Galochrom Chiral ION-QN & Chiral ION-QD

• Brochure

Weak Anion-Exchanger (WAX) stationary phases for reliable chiral separation of acidic compounds

Transform Your Chiral Analysis

Weak Anion-Exchanger (WAX) stationary phases for reliable chiral separation of acidic compounds One of the main challenges of today’s liquid chromatography is chiral separation of ionised and ionisable analytes, e.g., organic acids, amino acids, N-protected amino acids, amino acid mimics, etc. The most efficient approach to purify and resolve such troublesome racemates utilises ion exchange-type stationary phases that facilitate strong interactions between the chiral selector and the analyte.

Galochrom introduces its own generic series of weak anion-exchangers, based on tert-butyl-carbamoylated Cinchona alkaloids quinine (QN) and quinidine (QD). These chiral phases have demonstrated excellent selectivity and improved peak resolution, resulting in highly accurate and replicable analyses. Our innovative manufacturing and strict quality control ensure that these generic columns not only outperform commercial alternatives, but also meet your technical requirements.

Chiral ION-QN & Chiral ION-QD represent the most efficient approach to purify and resolve even the most challenging mixtures.

Applications

Chiral ION-QN & Chiral ION-QD are ideal for enantioseparations of:

• N-protected amino acids
• Aminophosphonic & Aminosulfonic acids
• Lactic & Thiolactic acids
• Clenbuterol & Thyroxine

2. Metrohm: Electrochemical Impedance Spectroscopy - Equivalent circuit models

• Technical note

Electrochemical Impedance Spectroscopy

Part 4 – Equivalent circuit models

The circuit elements which are described in Application Note AN-EIS-003 can be combined in series and in parallel to build equivalent circuit models which can then be used to model the various phenomena occurring at the electrochemical interface.

This seven-part series introduces EIS and covers basic theory, experimental setups, common equivalent circuits used for fitting data, and tips for improving the quality of the measured data and fitting. This Application Note (part 4) provides example equivalent circuit models produced from the elements discussed in part 3. These models are among the most commonly encountered within electrochemistry research. The associated Nyquist plot is also shown for each model discussed.

CONCLUSIONS

This Application Note shows how electrical elements can be arranged in order to build both simple and more complex equivalent circuits that can be used for fitting EIS data. The resulting Nyquist plots for all the equivalent circuits are shown as well.

3. Thermo Fisher Scientific: Developing an ion chromatography system

• Technical note

Introduction

Ion chromatography (IC) has become essential for analyzing ionic and small polar compounds. It has been applied in many areas, ranging from the analysis of drinking water, food and beverages, and cooling water to lithium-ion battery research, process quality assurance, and the presence of corrosives in liquified petroleum gas.

IC can trace its origins to work done at what would become Dionex Corporation in the mid-1970s with the introduction of the first ion chromatograph in 1975, the Dionex™ Model 10 IC system. This system had the essential elements of an IC system: a pump, separating column, eluent suppressor, conductivity detector, and data recorder (Figure 1).

This basic system provided adequate data, but several factors restricted sample throughput and required a considerable investment in labor and significant expertise to maintain. Column capacity and packed bed suppressor capacity were limited, and the instrument configuration was inflexible, constraining the type of samples that could be analyzed. Offline suppressor column regeneration was needed, the pressure tolerance was low, and the background conductivity was comparatively high. Furthermore, manual peak integration was required, eluent usage was significant, and there was substantial run-to-run variability. Since the Dionex Model 10 IC system, many innovations have been developed and incorporated into new systems to address these deficiencies. Additional advancements have enhanced robustness, reliability, user-friendliness, functional flexibility, and integrated data analysis. Ideally, an ion chromatograph will meet current customer demands while being adaptable to address potential future analytical needs.

Conclusion

The progression from the Dionex Model 10 IC system to the sophisticated Dionex Inuvion IC system highlights the significant advancements that have been made in the field of IC. These advancements have not only addressed previous limitations but also introduced new features and capabilities that significantly enhance the performance, reliability, and user-friendliness of IC systems. As a result, the Dionex Inuvion IC system represents the current pinnacle in the ongoing development of IC technology, setting a new standard for what can be achieved in the analysis of ionic and small polar compounds.

The Dionex Inuvion IC system is the result of state-of-the-art techniques and processes used to manufacture, design, and optimize essential hardware components such as pumps, instrument electronics, range-free detectors, and conductivity cells. This integration of advanced technology has resulted in a system that is not only reliable and robust but also flexible and user-friendly.

As we look to the future, the field of ion chromatography will continue to evolve with new challenges and opportunities on the horizon. The Dionex Inuvion IC system is well-positioned to meet these challenges, providing laboratories with a reliable and efficient solution for their analytical needs. In conclusion, the Dionex Inuvion IC system represents a significant achievement in ion chromatography, solidifying Thermo Fisher Scientific's position as a leader in the industry.

4. Waters Corporation: A High Throughput LC-MS Method for Cell Culture Media Nutrient and Metabolite Analysis Supporting Upstream Bioprocessing

• poster / ASMS

INTRODUCTION

A 9-minute rapid and direct liquid chromatography and mass spectrometry (LC-MS) analysis method for cell culture media (CCM) nutrients and metabolites covering 220+ compounds is described. The method is based on reversed phase chromatography where amino acids are directly detected without derivatization. This rapid method reduces turn-around time for monitoring and decision making using previously established user-friendly data review workflows and access to multivariate data analytics (MVDA). The method has been applied for the qualitative and quantitative determination of cell culture media nutrient and metabolite analysis in commercial cell culture media and spent media from process optimization in cNISTmAb production using NISTCHO cells. Monitoring of glucose directly from media using this method was also investigated and described.

CONCLUSION

• A rapid throughput method based on 9 min data acquisition is described for cell culture media nutrient and metabolite monitoring.
• The method uses less than 10 μL of spent media sample and has coverage of 220 compounds.
• Comparison with the previous 20 min method suggests the same high-quality data and method robustness, even when the analysis time is shortened by 50%.
• Combination of the rapid throughput method with Waters bioprocess walk-up solution² can enable analytical scientist and bioprocess engineers to obtain high quality data easily and routinely for upstream bioprocess optimization.

5. Shimadzu: Automatic Optimization of Gradient Conditions by AI Algorithm for Impurity Analysis

• Application

User Benefits

• The AI algorithm of LabSolutions MD can automatically optimize gradient conditions to greatly reduce labor of LC method
  development.
• Anyone can optimize gradient conditions, regardless of their experience in chromatography.
• Gradient conditions that meet the resolution criteria for specified peaks are automatically searched (e.g., principal component and its related impurities).

Introduction

In the typical LC method development, the process begins with “preparation” which includes mobile phase preparation, column installation, and creation of analysis schedules, then the analysis is started. After that, the acquired data is analyzed and “preparation” for the subsequent analysis is carried out, followed by starting the next analysis again. The method development progresses by repeating these processes, but in addition to the significant time required to repeatedly create analysis schedules, expertise in chromatography is necessary to explore optimal conditions based on data analysis. In other words, typical method development requires “human intervention”. Therefore, eliminating human involvement and automating such method development processes would be desirable to improve labor efficiency. This article introduces an example of automatic optimization of gradient conditions to separate montelukast (a small molecule drug) and its related impurities using LabSolutions MD (Technical Report C190-E309), a dedicated software for supporting method development.

Conclusion

Automatic optimization of gradient conditions using AI algorithm of LabSolutions MD was applied to montelukast and its related impurity. As a result, gradient conditions that met the criteria (“resolution for montelukast and related impurity > 3.0” and “elution time of the last peak < 15 minutes”) were successfully explored. This result indicates that significant labor saving in method development can be expected by LabSolutions MD. This article introduces an automatic optimization of gradient conditions in method development while LabSolutions MD also supports a series of workflow of method development, including the screening phase and robustness evaluation phase. For details, please refer to the Technical Report “Efficient Method Development Based on Analytical Quality by Design with LabSolutions MD Software (C190-E284)”.

6. Agilent Technologies: Improved LC/MS Performance to Determine Polar Nitrosamines Using the Agilent 1260 Infinity II Hybrid Multisampler

• Application

Abstract

This application note demonstrates the use of the Agilent 1260 Infinity II Hybrid Multisampler for the analysis of polar nitrosamines injected from organic solvents of high elution strength. The 1260 Infinity II Hybrid Multisampler is used under optimized feed speed conditions to trap and enrich the polar nitrosamines on the column. This avoids breakthrough and provides better peak shapes with more reliable quantification and improved detection limits.

Introduction

With the chemical synthesis of active pharmaceutical ingredients (APIs), impurities occur during chemical reactions. Genotoxic impurities (GTIs) are especially important because of their carcinogenic potential. To control the amount of GTIs, the U.S. Food and Drug Administration and the European Medicine Agency released guidelines for the maximum intake of GTIs with the daily dose of a drug depending upon the duration of application. According to these guidelines, the exposure to an individual genotoxic impurity must be below 1.5 μg/day for an application time longer than ten years.¹ In 2018, the drug Diovan was withdrawn from the market due to an increased amount of the nitrosamine impurity N-nitrosodimethylamine (NDMA) in the included API valsartan.^2,3 This application note describes the results achieved by the Agilent 1260 Infinity II hybrid injector for the analysis of nitrosamines injected from high organic solvents. The peak performance, like area precision, linearity, and sensitivity, will be discussed.

Conclusion

This application note describes the comparative measurement of nitrosamines using the Agilent 1260 Infinity II Hybrid Multisampler in feed injection mode and classical flow through injection mode. With the application of an optimized feed injection method, highly polar nitrosamines in a solvent of high eluting strength can be separated with good peak shapes. With classical flow through injection, massive peak broadening or even breakthrough were observed. Peak area RSD and LOQs are typically lower by a factor of 3 to 5 with feed injection.