News from LabRulezGCMS Library - Week 26, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 23rd June 2025? Check out new documents from the field of the gas phase, especially GC and GC/MS techniques!

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This week we bring you application note by Shimadzu, posters by Agilent Technologies / ASMS and Thermo Fisher Scientific / ASMS and presentation by William & Mary / MDCW!

1. Agilent Technologies / ASMS: Improved Determination of Polychlorinated Biphenyl Compounds by US EPA Method 1628

• Poster
• Full PDF for download

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 can be found in the air, water, and soil and have been known to bioaccumulate in marine life.

The EPA has recently developed a low-resolution mass spectrometry method that can calibrate 65 PCBs congeners and screens for all 209 using labeled PCB compounds for direct and indirect quantitation² . The 65 congeners are targeted for calibration and quantitation due to specific factors described in the method² . As with most EPA methods, the prescribed methodology utilizes helium as a carrier gas. The recommended column for this analysis makes adequate separation and quantitation more challenging. To achieve separation that meets the method criteria, the run time is over 40 minutes long. By using a column better suited for PCB congener separation and hydrogen as the carrier gas, superior separation can be achieved in under 20 minutes, resolving previously co-eluting analytes.

Experimental 

System configuration using hydrogen carrier gas 

The Agilent 8890/5977C GC/MSD equipped with the HydroInert Ion source was operated in selective ion monitoring (SIM) mode for this analysis.

Conclusions

Faster Analysis, Superior Separation Achieved 

• The DB-XLB column offers enhanced selectivity for PCB congeners, resulting in previously co-eluting congeners to separate. 
• Selectivity is easily achieved operating the MSD in SIM mode. 
• The method meets the 10ppb detection limit for all the quantified compounds.
• The HydroInert ion source allows hydrogen carrier gas to be used for more rapid analysis.

2. Shimadzu: Simultaneous Analysis of Synthetic Musk Compounds in Water Using a Triple Quadrupole GC-MS System

• Application note
• Full PDF for download

User Benefits:

• Using a GC-MS/MS, synthetic musk compounds in water can be accurately quantified with high sensitivity.
• Supporting effective environmental monitoring in water and risk assessment using GC-MS/MS

Synthetic musk compounds (SMCs) are synthetic organic substances designed as substitutes for natural musk and are widely used in various household products. During everyday activities such as showering and washing, these compounds are released into wastewater. However, current wastewater treatment processes cannot completely remove SMCs, allowing them to enter aquatic ecosystems. As highly bio-accumulative organic compounds, SMCs can cause both acute and chronic toxicity in aquatic organisms. They are also known to cause endocrine disruption when accumulated in the human body1-3) . Due to these potential risks, continuous monitoring of SMCs in water is essential. The main analytical methods for detecting SMCs in water include liquid-liquid extraction (LLE), solid-phase extraction (SPE), and solid-phase microextraction (SPME). Liquid-liquid extraction method requires a large amount of solvent and long preparation time but has the advantage of simultaneously extracting multiple organic compounds 4) . In this application news, 15 types of SMCs in water were simultaneously analyzed using the gas chromatography method with liquid-liquid extraction method.

Analytical conditions

In this newsletter, SMCs in water were analyzed using GCMSTQ8050 NX of SHIMADZU (Figure 1). The instrumental detailed analytical conditions of instrument and the MRM conditions for each compound were shown in Table 1 and 2, respectively.

Conclusions 

The simultaneous analysis of 15 SMCs in water was performed using the SHIMADZU GCMS-8050 NX system. The coefficient of determination(R2) of the calibration curve for all SMCs were 0.99 or higher. The LOD and LOQ were ranged from 0.003 to 0.020 ng/mL and 0.01 to 0.07 ng/mL, respectively. The recovery test results were between 86.3 % and 106.4 %, with a relative standard deviation (RSD) of 0.7 % to 4.2 %. This analytical method, using a GC-MS/MS system, provided reliable quantitative results for 15 synthetic musk compounds in water samples and demonstrated high sensitivity and efficiency.

3. Thermo Fisher Scientific / ASMS: Performance evaluation of GC-MS/MS for Dioxin analysis with amendments to EU Regulations 644/2017 and 771/2017 for food and feed 

• Poster
• Full PDF for download

Polychlorinated dibenzo-p-dioxins/furans (PCDD/F), or dioxins, are persistent organic pollutants (POPs) that can accumulate within food chains due to their chemical stability and high fat solubility, posing health risks to humans through food consumption¹ . Current regulations monitor food and feed for dioxins, with maximal allowable levels for PDCC/Fs in feedstuffs at the pg•g-1 concentration range² . However, a recent review process has proposed a reduction of up to 40% in these levels by 2024 for certain feed items, such as animal/milk/egg fats (1.0 pg•g-1), fish oil (3.5 pg•g-1), and fish feed (1.0 pg•g-1)³ . Since 2014, the European Commission has permitted the use of gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) for food and feed analysis as an alternative to GC-high resolution mass spectrometry (HRMS)^4,5 . With the proposed reduction in maximum limits, the performance of current instrumentation to achieve these targeted limits must be assessed.

Laboratories face challenges in maintaining consistent sensitivity to detect trace levels of dioxins in complex food matrices and in reporting various regulatory requirements for PCDD/ F analysis^6,7 . This study used the Thermo ScientificTM TSQTM 9610 triple quadrupole GC-MS/ MS system with the NeverVentTM advanced electron ionization (AEI) source to demonstrate compliance with the proposed regulatory limits for PCDD/F in food and feed samples. The aim was to ensure consistency with previously determined concentrations of PCDD/F in food and feed matrices and meet current compliance with the EU regulations.

Materials and methods

Data was acquired, processed, and reported using the Thermo Scientific Chromeleon Chromatography Data System (CDS) software, version 7.3. Integrated instrument control ensures full automated setup of the Dioxin analytical workflow through the eWorkflow which provides optimized instrument / quantification methods, view settings for time efficient data evaluation and customizable report templates. Isotopic dilution quantification is performed automatically in real time with the incorporated custom variable and formula functionality eliminating the need for exporting to external software packages.

Conclusions 

The results of these comprehensive experiments demonstrate that the TSQ 9610GC-MS/MS system, configured with the NeverVent AEI source and controlled using Chromeleon CDS software together with the Dioxin eWorkflow, can deliver reliable regulatory compliant performance for the quantification and confirmation ofPCDD/Fs food and feedstuffs: 

• Fentogram level sensitivity performance for ultra trace level determination of PCDD/F within food and feed samples 
• Check standard performance was within quantitation and ion ratio thresholds for regulatory method compliance at femtogram levels. 
• Accurate and precise quantitation at both current and newly adopted maximum limits for PCDD/F in food and feed. 
• Chromeleon CDS software, version 7.3, provides an integrated platform, with the ability to automatically setup, easily acquire, process and report compliant data in a fully regulated environment, eliminating the need for using external spreadsheet programs. 
• Chromeleon eWorkflows, available from Thermo Scientific also provide error-free execution of each analysis to meet standard operating procedure (SOP) requirements, further simplifying the user

4. William & Mary / MDCW: Method optimization of fingermark residue using comprehensive two-dimensional gas chromatography 

• Presentation
• Full PDF for download

Fingermarks—smudged or incomplete fingerprints—may lack value for direct identification but can still offer critical information through their chemical residue. This study explores the potential of nontargeted chemical analysis of fingermark residue to determine donor characteristics such as sex and age. Using comprehensive two-dimensional gas chromatography (GC×GC), the team sought to enhance analytical resolution and method efficiency.

Experimental Approach

Researchers first collected fingermark residue using cotton swab extraction, followed by centrifugation and sample preparation. A GC×GC method was optimized by adjusting parameters like modulation period, hot pulse time, oven hold times, and ramp rate. Multiple method configurations were tested for chromatographic resolution, and the optimized helium-based method was later translated for use with hydrogen carrier gas using modeling tools.

Results

Method optimization led to significant improvements in peak separation, enabling identification of various compound classes including sterols, fatty acid methyl esters, fatty alcohols, and steroids. Additionally, unexpected anthropogenic substances such as sunscreen agents and plasticizers were detected. Hydrogen-based methods were able to achieve comparable separation quality, with the “H₂ Translate” method offering the highest number of identifiable peaks.

Conclusion

This study demonstrates that nontargeted GC×GC analysis is effective for resolving both endogenous and exogenous compounds in fingermark residue. The optimized methods not only improve forensic chemical profiling but also support a successful transition from helium to hydrogen as a carrier gas—promoting sustainability without compromising analytical performance.