News from LabRulezGCMS Library - Week 8, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezGCMS Library in the week of 17th February 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 notes by Agilent Technologies  and Shimadzu and product spotlight by Thermo Fisher Scientific!

1. Agilent Technologies: Extractable Pollutants from Microplastics to Vegetables: Incorporation to the Food Chain

Using static headspace GC/MS with the Agilent 8890 GC and 5977B GC/MSD

• Application note
• Full PDF for download

Most studies of organic pollutants in vegetables focus on persistent organic pollutants (POPs)^10,11, which are extracted from samples and usually monitored by liquid chromatography (LC).¹² However, the accumulation of MP-associated pollutants in vegetables has hardly been evaluated.

This application note presents:

1. A developed and validated approach to the targeted and
   untargeted analyses of MP-associated pollutants found in vegetables
2. Quantitation of MP pollutants
3. Assessment of the influence of vegetable type (edible- versus nonedible-roots) on the intake of MP-associated pollutants
4. The accumulation and environmental migration pathways of the MP pollutants

In this application note, an SHS-GC/MS method involving a static headspace coupled to an 8890 GC and 5977B GC/MSD was used for the evaluation of volatile extractables from plastic residues present in vegetable matrices. This technique is well suited to extract volatile compounds from different samples due to its simplicity, automation, speed, low cost, and minimal sample preparation requirements.^13–15 Additionally, the application of MS in combination with a spectral deconvolution and retention indices (RIs) enabled advanced detection and identification of volatile MPassociated pollutants in vegetable matrices. 

Conclusion

A straightforward, reliable, and robust SHS-GC/MS methodology using an Agilent 8890 GC and an Agilent 5977B GC/MSD was developed to identify and quantify plasticassociated pollutants in vegetable samples. The method represents a preliminary approach to assess the impact of agricultural MP contamination on food. The obtained data add new information to the mobility of MP leachates from agricultural soils to vegetables. The application of chemometrics to the dataset acquired from the SHS-GC/MS analysis has demonstrated that the accumulation of these organic pollutants was higher in edibleroot than nonedible-root vegetables. The main contributors to this differentiation were 2,4-di-tert-butylphenol, cumene, 2-tert-butyl-4 methylphenol, and 2,4-dimethylphenol, which are chemicals associated with plastic contamination. Specifically, cumene may be related to polystyrene (PS) pollution.

A total of 92 putative compounds were accurately identified using spectral deconvolution retention indices (RIs). In the samples, plastic-associated compounds were quantified. Their contents varied from 0.14 to 28,800 ng/g for 2,4-di-tert-butylphenol and p,α-dimethylstyrene, respectively. The presence of phenylacetaldehyde in all the samples, as well as styrene, cumene, and p,α-dimethylstyrene in some of them, indicated PS contamination. Other compounds found in the studied vegetables, such as xylene isomers and ethylbenzene, highlighted potential contamination of other polymeric materials like polyvinyl chloride (PVC) or polyethylene terephthalate (PET).

2. Shimadzu: Analysis of Essential Oil Using GC-MS/FID Detector Splitting System

• Application note
• Full PDF for download

User Benefits

• The detector splitting system allows for simultaneous acquisition of MS and FID data in a single measurement.
• Even complex samples can undergo simplified statistical analysis using the eMSTAT Solution^TM.
• The combination of the compact Brevis^TM GC-2050 and GCMS-QP2050 enables space-saving in the laboratory.

In this application, five types of Hinoki oils, including Hinoki oil made by our company and Hinoki oils from different regions, were analyzed using the detector splitting system between MS and FID. The results from MS were compared using eMSTAT Solution to analyze the composition of the components. Additionally, the quantification of δ Cadinene, an important aromatic component that is a sesquiterpene was conducted using FID, which showed high calibration linearity over a wide concentration range. Furthermore, with a compact width of approximately 63 cm, the device configuration of Brevis GC-2050 + GCMS-QP2050 not only contributes to space-saving in the lab but also demonstrates high analytical performance.

Essential Oil Analysis Using GC-MS/FID

In quality control (QC) of fragrances like Hinoki oil, where a wide concentration range is typically expected, GC-FID, which provides detector response over a broad range, is commonly used. By comparing the chromatogram shapes of product samples obtained during the production process with approved reference samples, the component profile is confirmed. However, in the case of Hinoki oil containing numerous components, qualitative analysis of each peak becomes challenging with an FID detector. Therefore, by using the detectorsplitting system between MS and FID, it is possible to obtain data from both MS and FID simultaneously in a single measurement. This allows for the usual confirmation of chromatogram shapes with FID and enables qualitative analysis with MS when unknown components are detected.

System Configuration and Analysis Conditions

The system configuration and analysis conditions are shown in Table 1 and 2, respectively In this analysis, SMI (Smart Micro Inert) FLOW DEVICE 2-Way Splitter for detector splitting was used (Fig. 1). The SMI FLOW DEVICE is a capillary flow device for analysis with features such as low leakage, low dead volume, low heat capacity, and inertness. This allows for the analysis of highly adsorptive components. We adjusted the inner diameter of the resistors used for MS/FID detector Splitting, as well as the pressure of the AUX-APC (Digital Flow Controller), to set the split ratio at approximately 1:3 for MS:FID. By using eMSTAT Solution for analysis, we visually grasped the differences in component characteristics of each Hinoki oil and identified the compounds contributing to those differences.

Conclusion

Five different types of Hinoki oils were analyzed using a detector splitting system with MS and FID. When conducting multivariate analysis with the results from MS using eMSTAT Solution, it was possible to visually capture the differences in component characteristics. It was revealed that (-)-Borneol is a characteristic component of Shimadzu oil. Additionally, accurate quantification of δ-Cadinene, which varies significantly in concentration among samples, was achieved using FID.

3. Thermo Fisher Scientific: Fully automated method implementation for compliant analysis of polychlorinated dibenzodioxins/furans by GC-MS/MS

• Other
• Full PDF for download

Performance-based methodology for dioxin analysis is applied within the EU to ensure accurate reporting of dioxin levels within food and feed. Results are evaluated according to strict quality control and reporting criteria. For analytical testing laboratories, this often means a significant time investment for adoption and implementation of the methodology for dioxin analysis, as well as a requirement for highly skilled operators. Even for laboratories experienced with GC-MS-based test procedures, the addition of dioxin testing to the overall portfolio is demanding. To simplify this process, a dedicated eWorkflow™ template is available within the Thermo Scientific™ Chromeleon™ Chromatography Data System. This eWorkflow template is available for the Thermo Scientific™ TSQ™ 9610 triple quadrupole GC-MS/MS system and is free to download from the Thermo Scientific™ AppsLab™ Library of Analytical Applications (Dioxin eWorkflow). 

Processing methods within the Dioxin eWorkflow template use isotopic dilution for quantitation, allowing users to perform data acquisition and real-time quantitation within the same software. Spiking levels of both syringe and internal standard can be defined per injection, permitting samples spiked with different levels of internal or syringe standard concentration to be analyzed in a single sequence. This can be seen in Figure 3 where internal standard concentration level within the sequence is defined at different levels for calibration standards (i.e., PCDD/F CS1), check standards (LOQ, LOQ/2, LOQ/4), and blank/sample injections (Sample).

The Dioxin eWorkflow template allows analytical testing laboratories to easily implement compliant analytical methodology for dioxin analysis. It delivers validated data acquisition/processing methods and reporting templates for dioxin analysis, helping remove time-consuming steps around method development and data processing.

Included within the Dioxin eWorkflow template:

• Injection sequence templates with pre-optimized analytical parameters for method injection and data acquisition.
• Incorporation of isotopic dilution quantitation, removing the need for additional software or script writing to perform data calculations.
• Interactive tables and charts to facilitate quick data evaluation for compliance purposes.
• Fully customizable data evaluation and report layout templates based on the analyst’s needs.