News from LabRulezLCMS Library - Week 6, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 3rd February 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!

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This week we bring you tech. note by Agilent Technologies, applications by Shimadzu, Thermo Fisher Scientific, Metrohm, and Poster by Waters Corporation!

1. Simultaneous Determination of Five Genotoxic Aryl Sulfonate Impurities in Pharmaceuticals by LCMS-2050

• Application note
• Full PDF for download

User Benefit

• A novel method for determining the content of five genotoxic aromatic sulfonate impurities in drugs was established by using LCMS-2050 single quadrupole mass spectrometer.
• The pretreatment of this method was simple, and it had a wide linear range and a high accuracy rate.

Introduction

Genotoxic impurities (GTIs) refer to substances that directly or indirectly damage cellular DNA, generating gene mutations or in vivo mutagenesis. GITs may can cause damage to human genetic material at extremely low concentrations, which in turn leads to gene mutations and promotes the occurrence of tumors. Because of the potential risks of GITs, it is essential to monitor any potentially existing genotoxic impurities in active pharmaceutical ingredients or medicinal products.

In the pharmaceutical industry, when drug active ingredients exist in the forms of alkyl sulfonates, benzenesulfonates, p-toluenesulfonates, and hydroxyethyl sulfonates or sulfonic acid reagents are utilized in the drug synthesis process, sulfonate esters are regarded as potential GTIs. GTIs of sulfonate esters can be classified as alkyl sulfonate esters and aryl sulfonate esters based on different substituents.

Previously, relevant literature has reported quantitative detection methods for some GTIs of sulfonate esters, such as GC-MS, GC-FID, LC-MS/MS, and complex derivatization treatment of samples might be necessary. In this study, LC-MS was mainly utilized for the quantitative analysis of five GTIs of aryl sulfonate esters. This method features simple pretreatment and high accuracy, which can offer a reference for the detection of genotoxic impurities of aryl sulfonate esters in drugs.

Conclusion

A novel method for determining the content of five genotoxic impurity aryl sulfonates in drugs was established by using the LCMS-2050. Within the concentration range of 5 - 500 μg/L, the correlation coefficients of the five genotoxic impurity aryl sulfonates were all greater than 0.994. When a mixed standard solution of three concentrations was added to the drugs, the recovery rates of each component ranged from 110.5% to 115.3%. This method features simple pretreatment, excellent specificity and high sensitivity, and can provide a reference for the determination of the content of five genotoxic impurities aryl sulfonates in drugs.

2. Method Transfer from an Agilent 1100 Series Quaternary LC to an Agilent 1260 Infinity III LC

• Technical Overview
• Full PDF for download

Proof of equivalency for the transfer of conventional LC methods

Method transfer from legacy equipment to new instruments, such as the Agilent 1260 Infinity III LC, is an important topic for all laboratories throughout different industries. Seamless method transfer ensures that the same methods can still be used, which ensures business continuity and reduced regulatory and financial risks.

This technical overview demonstrates method transfer from an Agilent 1100 Series Quaternary LC to an Agilent 1260 Infinity III LC for conventional LC methods covering diverse gradient conditions. Equivalent results are obtained, which proves that seamless method transfer can be expected for typical, robust, conventional LC methods. In terms of retention time precision, the 1260 Infinity III LC outperforms the 1100 LC, leading to higher trust in the data.

Introduction

Method transfer is an important topic for all laboratories throughout different industries, where HPLC methods are transferred between departments and locations as well as between different LC instruments.¹ For validated methods in the pharmaceutical industry, method transferability is compulsory.

Method transfer, or the transfer of analytical procedures from one laboratory to another in the pharmaceutical industry requires a documented process that requires comparative testing.² One example for instrument-to-instrument method transfer is the transfer of conventional LC methods from legacy equipment to new instruments such as a 1260 Infinity III LC.

This technical overview demonstrates method transfer from a 1100 Series Quaternary LC to a 1260 Infinity III LC for conventional LC methods. Several methods were chosen that cover diverse gradient conditions including challenging conditions such as a shallow gradient and a gradient starting at a composition extreme. This should prove that equivalent results are obtained when transferring methods from a broad application space of conventional LC methods from the 1100 Series Quaternary LC to the 1260 Infinity III LC.

Conclusion

The transfer of conventional LC methods covering diverse gradient conditions from an Agilent 1100 Series Quaternary LC to an Agilent 1260 Infinity III LC leads to equivalent results, thereby proving that seamless method transfer can be expected for typical, robust, conventional LC methods. In terms of retention time precision, the 1260 Infinity III LC outperforms the 1100 LC, leading to a higher trust in the data.

3. Development of Separation Methods for GLP-1 Synthetic Peptides Utilizing a Systematic Protocol and MaxPeak High Performance Surface Technology

• Poster / HPLC Symposium
• Full PDF for download

Peptides offer higher specificity than small molecules, and low immunogenicity which makes them excellent candidates for new medications. Specifically synthetic peptides produced through solid phase peptide synthesis allow for more control with more predictable impurities with a relatively low manufacturing cost.

An excellent example of upcoming synthetic peptide drugs is Glucagon-Like Peptide-1 Agonists (GLP-1s) which are prescribed for the treatment and management of obesity and type-II diabetes1. Recently, GLP-1 drugs such as semaglutide, have boomed in popularity as a weight management treatment after success in clinical trials.2 Given the prevalence of GLP-1s, it is important that the quality control for this class of pharmaceuticals is supported by versatile, sensitive, and reproducible chromatography methods.

Here we address these needs and developed a single HLPC-UV/MS method for the analysis of a variety of GLP-1s. The experiment was based around a systematic protocol which was key in helping to identify high-risk factors and to shorten the method development time. Beyond this MaxPeak high performance (HPS) technology was used to improve chromatographic performance.

Conslusion

The thoughought assessment of the risk before conduction the development of a separation method allowed for the ccreation of a more quality method while reducing time. Asessing the high risk variables showed ther benefit in MaxPeak HPS technology when working with these compounds. MaxPeak HPS technology

4. Quantifying impurities in cationic lipids raw materials with the inverse gradient method using LC-CAD-MS

• Application note
• Full PDF for download

Application benefits

• Enable the quantification of impurities even in the absence of specific reference standards
• Use a single quadrupole mass spectrometer to match impurities based on their retention time and molecular masses
• Use an inverse gradient with Charged Aerosol Detector (CAD) to enable accurate surrogate quantitation when there is large difference in retention times between the lipid standard and its impurities, even in the absence of impurity standards
• Confirm the unit mass of both the lipid standard and its associated impurities using the correlation of CAD and ISQ channels

Goal

• Provide instructions, methodologies, and recommended techniques to improve quantification of impurities in cationic lipid components
• Use the Thermo Scientific™ Vanquish™ Flex Inverse Gradient UHPLC System coupled to a Thermo Scientific™ Vanquish™ Charged Aerosol Detetor to provide more accurate estimated quantitation of cationic lipid impurities without the need for reference standards

Conclusion

In this study, we have developed an inverse gradient quantification method for cationic lipids impurity analysis when impurity reference standards are not available. For further identification of lipid impurities, Application Note 002455 can be referenced.

• The impurity amount can be automatically estimated using another peak or peak group within the same run for this surrogate quantitation in Chromeleon CDS.
• Both inverse gradient configuration and method can be automatically generated via the wizard.
• When there is a significant difference in retention times between the lipid standard and its impurities, using an inverse gradient provides more accurate estimated quantitation than a conventional gradient method.
• The use of the ISQ EM MS in conjunction with CAD allowed for confirmation of the m/z of the lipid raw material as well as determination of the m/z for the unknown impurities.

5. Using a portable standalone system for easy fermentation monitoring

• Application note
• Full PDF for download

In-situ measurements of lactic acid in beer using screen-printed electrodes (SPEs)

Lactic acid (2-hydroxypropanoic acid) is primarily found in sour dairy products. In beer, the presence of lactic acid contributes to its acidity and lactic aromas, and usually appears as the result of fermentation with lactic acid bacteria. These bacteria may be purposely introduced to the wort, or they can also appear as a result of an infection.

Although lactic acid is essential in beer up to a certain amount, in excess it is considered a defect. Its perception threshold is 0.0044 mol/L. However, in some lambic-type beers, the lactic acid concentration can reach levels higher than 0.0333 mol/L.

In this Application Note, an enzymatic sensor based on a screen-printed electrode is used to measure lactic acid in commercial beers as a proof of concept for its potential application during fermentation monitoring.

Conclusion

In this study, an electrochemical biosensor for the detection of lactic acid in beer is proposed. The sample with the electrochemical method proposed only needs to be diluted 1:10 with a solution of 0.1 mol/L Tris-NO₃ at pH 7.2. Using a simple amperometric assay, it is possible in 75 s to measure the amount of lactic acid in a beer sample without any pretreatment. Measurements obtained are similar to those taken with a traditional L-Lactate Assay kit and non-portable optical devices