News from LabRulezGCMS Library Week 29, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 15th July 2024? Check out new documents from the field of gas phase, especially GC and GC/MS techniques!

👉 SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT GCMS AND RELATED TECHNIQUES

👉 Need info about different analytical techniques? Peek into LabRulezLCMS or LabRulezICPMS libraries.

This week we bring to you poster presentations from ASMS 2024 by LECO, Agilent Technologies, Shimadzu, and Thermo Fisher Scientific!

1. LECO: Non-Targeted Analysis of Complex Environmental Samples Using Thermal Desorption, Multidimensional Gas Chromatography, Multi-Mode Ionization Methods, and High-Resolution Time-of-Flight Mass Spectrometry

• poster - ASMS 2024

Introduction

• Confident analysis of environmental samples (e.g., air, water, dust/soil) is critical for the monitoring of harmful substances such as persistent organic pollutants
• Many of these harmful chemical substances have been classified as carcinogens and endocrine disruptors
• Study Objective: To use GCxGC-HRTOFMS for the analysis of complex environmental samples.

Challenge: Complex environmental samples are difficult to analyze

• Very large number of sample constituents
• Wide concentration range
• Varying physiochemical properties

Summary:

• HRT and MMS technology are powerful tools for the analysis of complex environmental samples (dust, food, air)
• Compounds were annotated using:
  • Database comparisons
  • Formula determinations using high-resolution accurate mass ions
  • Chemical ionization data resulted in increased confidence for compound annotation

2. Agilent Technologies: Two Methods to Perform the New US EPA Method 1628 with GC/MSD: Traditional Helium Carrier Gas and Hydrogen Carrier Gas

• Poster - ASMS 2024

Introduction: Polychlorinated Biphenyl (PCBs) and the Environment

Polychlorinated Biphenyls (PCBs) are synthesized compounds that belong to the chlorinated hydrocarbon family of compounds. PCBs were used in a variety of industrial applications such as electrical components, plasticizers and pigments/dyes, until they were banned in 1979 by the Toxic Substances Control Act (TSCA)1. PCBs are considered to persistent organic pollutants (POPs) as they do not easily degrade in the environment. PCBs, which are classified as probable human carcinogens, can be found in the air, water, and soil and have been known to bioaccumulate in marine life. Overall, users of this whole validated procedure profit from easy and standardized handling, the precise determination of the analytes, automatic eluent roduction, calibration, and results calculation, low maintenance, and a single-manufacturer setup.

Conclusions: Two Robust methods for EPA Method 1628 was developed to analyze 209 native and 35 labeled PCB Congeners

• Using EPA Method 1628 guidelines and requirements, a robust method was developed with helium carrier gas.
• Using MassHunter method translator, a faster method that meets EPA Method 1628 guidelines was developed using Hydrogen carrier gas.
• Both methods can detect and quantitate PCB compound down to the single digit ppb levels.

3. Agilent Technologies: Analysis of Essential Oils Using a Comprehensive GCxGC with a Reverse Flow Modulator Combined with High Resolution GC/MS

• poster - ASMS 2024

Introduction: Essential oils are typically analyzed to determine their chemical composition contributing to flavor and quality as well as to evaluate their authenticity and identify adulterants. Essential oils are often complex samples with high number of volatile and semi-volatile components that include many isomers with highly similar spectra and close Retention Indices (RIs) when separated on a single column. Hence, a comprehensive GCxGC approach is preferable to achieve an appropriate chromatographic separation for this sample matrix. In this study we used comprehensive GCxGC coupled to a high-resolution accurate mass GC/MS to identify the essential oil components. Here we also investigate approaches for comparison of the complex GCxGC essential oil data.

Conclusions:

• Several comprehensive GCxGC configurations and method using the high-resolution GC/Q-TOF and RFM were developed and optimized using a diesel sample.
• Essential oils were analyzed using the optimized GCxGC approach, and the workflows for compound identification and statistical analysis were evaluated.

4. Shimadzu: Ultra-sensitive dynamic headspace GC-MS/MS method for trace level quantitation of Nitrosamines in Deferiprone API

• Poster - ASMS 2024

Introduction: Regulatory bodies related to pharmaceutical industry have extensively investigated the presence of genotoxic impurities, called Nitrosamines (NSA), in many drugs. Deferiprone is an iron chelator used to treat patients with transfusional iron overload caused by thalassemia syndromes. This drug is admired in high dose with long term treatment. Hence it is imperative to make Deferiprone drug available with safe levels of NSA.

Pharmaceutical drug product which contains Deferiprone, is supposed to consume for a longer time. Maximum daily intake is of 99 mg/kg/day. Considering worst case scenario, calculated Maximum Daily Dose (MDD) will be 9000 mg/day when weight of the patient as 90 kg. Hence, it is imperative to determine NSA with Limit of Quantitation (LOQ) < 0.1 ppb. Limits were calculated as per MDD of 9000 mg / day and reported in Table-1 with established LOQ’s for each NSA impurity. Developing method for determining total NSA at such low level in Active Pharmaceutical Ingredient (API) & Finish Dosage Form (FDF) creates challenges in pharmaceutical industry.

This poster describes a validated dynamic headspace GC-MS/MS procedure for quantification of various NSAs like N-nitroso-dimethylamine (NDMA), N-nitroso-diethylamine (NDEA), N-nitroso-ethylisopropylamine (NEIPA), N-nitroso-diisopropylamine (NDIPA), N-nitroso-dipropylamine (NDPA), and Nnitroso-dibutylamine (NDBA) in Deferiprone Active Pharmaceutical Ingredient (API).

Conclusion:

• Dynamic headspace mode, seamlessly meet the current regulatory limits, delivering high sensitivity compared to static headspace as well as liquid injection mode for nitrosamines analysis.
• Shimadzu GCMS-TQ8050 NX has features like a highly efficient shielded detector and superior noise reduction technology enhances sensitivity and enables quantitation of nitrosamines even at trace levels.

5. Shimadzu: Simultaneous determination of known and unknown Extractables in pharmaceuticals packaging material by tandem mass spectrometry using Scan-MRM mode

• Poster - ASMS 2024

Introduction: The purpose of Extractable & Leachable (E&L) studies in the regulatory references, is to identify the traces of potential chemical substances. Because these substances may be harmful to patient due to their toxicity, or the activity of drug product may impact because of their presence. Hence, to ensure the safety and efficacy of the drug till its shelf-life period, E&L study plays an important role. Extractables are organic or inorganic entities which are released from container closure system (CCS) into an extraction medium under laboratory condition. Whereas, leachable are the foreign organic or inorganic chemical substances which are present in the packaged drug product during normal as well as accelerated stability conditions.

Samples of CCS will be used for identification of extractables. However, packaged drug product sample will be used for the evaluation of leachable. Ophthalmic drug product packaging material was used for this study (Figure 1) and the analysis was carried out on Shimadzu triple quadrupole system GCMS-TQ8040 NX equipment (Figure 2).

Conclusion:

• The migration of extractables from the CCS includes a wide range of compounds. Highly sensitive and robust techniques is required for detection at trace level. Also, Data need to be acquired in both SCAN and SIM/MRM modes to detect known and unknown extractables simultaneously without affecting sensitivity.
• Shimadzu’s GCMS TQ-8040 NX triple quadrupole ultra fast mass spectrometer offers a SCAN speed of 20,000 amu/sec, 800 MRM transitions per second along with Advanced Scan Speed Protocol (ASSP) function, facilitates detection and identification extractables even at trace levels.

6. Thermo Fisher Scientific: Utilizing cost effective helium saving technology for low level quantitation of Polychlorinated dibenzo-p- dioxins/furans using gas chromatograph mass spectrometry

• Poster - ASMS 2024

Abstract

• Purpose: To demonstrate high sensitivity and robustness of a cost-effective and sustainable Helium saving injector for the analysis of polychlorinated dibenzo-pdioxins/furans (PCDD/PCDF).
• Methods: Sample analysis was carried out on the Thermo Scientific TSQ 9610 GC-MS/MS equipped with the new Thermo Scientific iConnect HeSaver-H2Safer split/splitless (SSL) injector. A sample volume of 1.5 μL was injected for chromatographic separation using a TG-Dioxin (60 m × 0.25 mm, 0.25 μm) capillary GC column with previously described conditions.1The GC-MS/MS system was equipped with an advanced electron ionization (AEI) source to increase sensitivity for analyte detection. Quantification was performed using isotopic dilution in Thermo Scientific Chromeleon Chromatography Data System software using the Dioxin Analyzer workflow.
• Results: The He saver demonstrated excellent robustness, precision, and sensitivity for PCDD/F analysis in soil extracts (analyzed with no prior clean-up) at fg levels while consuming 8 times less helium compared to the standard SSL injector.