News from LabRulezLCMS Library - Week 41, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 6th October 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 other document by Agilent Technologies and posters by Shimadzu / AOAC, Thermo Fisher Scientific / ASMS and Waters Corporation / AOAC!

1. Agilent Technologies: PFAS Food Legislation Overview

• Other document
• Full PDF for download

This Agilent Technologies eBook provides an overview of global PFAS (per- and polyfluoroalkyl substances) regulations and analytical methods for monitoring these compounds in food, beverages, and food-contact materials. PFAS are synthetic chemicals valued for their water- and grease-resistant properties but are highly persistent and bioaccumulative. Their potential health risks—including immune suppression, elevated cholesterol, liver enzyme changes, and developmental effects—have prompted worldwide regulatory action to limit exposure through food and packaging.

In the European Union, Regulation (EU) 2023/915 establishes maximum allowable levels of PFAS in various food products (e.g., meat, fish, eggs), ranging from 0.2 to 8 µg/kg depending on the matrix. Recommendation (EU) 2022/1431 encourages member states to collect PFAS occurrence data and harmonize testing methods, while the upcoming Packaging and Packaging Waste Regulation (PPWR 2025/40) will, from August 2026, limit PFAS in food packaging to 25 ppb per compound and 250 ppb total. Analytical testing across Europe relies primarily on liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS), which provides the ppb-to-ppt sensitivity needed for regulatory compliance.

In the United States, the framework combines federal, state, and industry standards. The USDA CLG-PFAS 2.04 method employs UHPLC/MS/MS to detect 16 PFAS in animal tissues, while the FDA C-010.03 method quantifies 30 PFAS in food and feed using solid-phase extraction (SPE) followed by LC/MS/MS. The AOAC SMPR 2023.003 standard defines performance criteria for PFAS testing across multiple food categories, ensuring validated and reproducible results. Several U.S. states—including Maine, California, and Washington—have also enacted specific limits for PFAS in meat, milk, and food-contact packaging.

In China, national standard GB 5009.253-2016 specifies the determination of PFOS and PFOA in animal-derived foods via isotope-dilution LC/MS/MS. A new draft revision expands testing to 30 PFAS compounds (including isomers) across broader food matrices such as fish, vegetables, and milk. Chinese authorities have also introduced bans and restrictions on PFOS, PFOA, and PFHxS production and use, along with environmental management and disposal requirements.

Agilent offers comprehensive PFAS testing solutions for food laboratories, including robust HPLC and LC/MS instrumentation, validated methodologies aligned with EPA, EU, and ASTM standards, and a curated PFAS MRM database. The portfolio also features Captiva EMR PFAS Food cartridges pre-tested for background contamination, certified PFAS standards, and data-handling tools such as Agilent MassHunter and SLIMS. Together, these workflows enable reliable PFAS quantification, reduced contamination risk, and full compliance with international food-safety legislation.

2. Shimadzu / AOAC: Reliable and direct quantitative analysis of multi-mycotoxins in animal feed by using Shimadzu LCMS-8050RX

• Poster
• Full PDF for download

Mycotoxins are toxic compounds produced by moulds that contaminate crops such as cereals, nuts, spices, dried fruits, apples, and coffee especially under warm, humid conditions. These chemically stable toxins can persist through food processing and pose serious health risks to humans and animals, ranging from acute poisoning to cancer and immunosuppressive. Among the many identified toxic compounds, Aflatoxins, Ochratoxin A, Fumonisins, T-2, Zearalenone, and Deoxynivalenol (DON) (Figure 1) are of particular concern. These are the most studied and regulated due to their significant impact on human and animal health, making their testing critically important. While conventional testing methods (HPLC-UV/FLD) are still common, regulatory focus is shifting toward LC-MS/MS testing due to its sensitivity and specificity.

The European Committee for Standardization (CEN), under the M/520 mandate, is developing standardized methods for this purpose. Mycotoxins are generally extracted via liquid–liquid (for milk, wine, juices) or solid–liquid extraction (for cereals, dried fruits, spices, feed), typically using acidic buffers. In this study, we developed a fast, highthroughput LC-MS/MS method for multi-mycotoxin detection in animal feed using the Shimadzu LCMS8050RX (Figure 2). MRM based quantitative method was developed using Shim-pack GIST C18-AQ HPLC column with an aim to achieve improved peak separation and required sensitivities for the compounds under study. A matrix-matched calibration curve (0.5–50.0 ppb) showed accuracy between 80–120 %, and recoveries (at 2.5 and 5.0 ppb) were 70–120 %, complying with SANTE guidelines[1] .

Materials and method

LC-MS/MS analysis

• UHPLC: Nexera X3
• MS: LCMS-8050RX

Conclusion 

• Average recovery values for multi-mycotoxins in animal feed sample were found to be within the acceptance criteria as per the SANTE/12682/2019 guidelines. 
• The results obtained at 2.5 ppb and 5.0 ppb concentration level were accurate, repeatable and reproducible with RSD less than 20 %.
• A simple liquid-liquid extraction method has been successfully developed and validated for the simultaneous quantification of nine mycotoxins in a single run.

3. Thermo Fisher Scientific / ASMS: High-throughput proteomics using narrow window DIA on the Orbitrap Astral Zoom MS

• Poster
• Full PDF for download

The recently introduced Orbitrap Astral mass spectrometer has significantly expanded the scale and scope of proteomics experiments, advancing discovery and translational research. Building on this innovation, we demonstrate the performance of the next evolution of the platform, the Orbitrap Astral Zoom mass spectrometer, at throughputs ranging from 30 to 300 samples-per-day (SPD) analysing a HeLa digest using narrow window data-independent (nDIA) acquisition. The novel instrument features a higher acquisition rate (270 Hz vs. 200 Hz) achieved through improved ion optics settling times and faster ion transfers, increased sensitivity via pre-accumulation, and deeper coverage through enhanced spectral processing, among other improvements. Comparative analysis with the Orbitrap Astral MS reveals further improvements in peptide and protein group identifications enabling even deeper coverage at high throughput whilst maintaining precise quantitation.

Methods

HeLa digest standard measured on Orbitrap Astral Zoom MS and Thermo Scientific Orbitrap Astral MS coupled to Thermo Scientific Vanquish Neo UHPLC utilizing 30-300 samples-per-day (SPD) LC-MS methods

Conclusions 

The novel Orbitrap Astral Zoom mass spectrometer is, among its broad and comprehensive range of applications, an excellent instrument for high-throughput proteomics. 

• High-throughput nDIA on the Orbitrap Astral Zoom MS generates deep coverage of proteomes
•  The novel Orbitrap Astral Zoom MS further pushes the boundaries in terms of quantity and quality of identifications 
• The Orbitrap Astral Zoom MS enables precise quantitation with full flexibility to focus on MS2-based quantitation

4. Waters Corporation / AOAC: Integration of Ultra-short Chain PFAS Into Routine Analysis Methods: Addressing Retention and Confirmatory Ions

• Poster
• Full PDF for download

The poster presents a novel LC-MS/MS workflow enabling simultaneous quantification and confirmation of ultra-short through long-chain PFAS in a single analysis. The work was conducted using a Waters ACQUITY Premier LC system equipped with a PFAS kit, Atlantis Premier BEH C18 AX mixed-mode column, and a Xevo TQ Absolute tandem mass spectrometer with waters_connect software for quantitation.

The study addresses two analytical challenges: (1) the poor chromatographic retention of ultra-short chain PFAS (e.g., TFA, PFPrA) on conventional reverse-phase columns and (2) the absence of confirmatory ions for some short-chain PFAS, which typically produce limited fragment ions. Using the Atlantis Premier BEH C18 AX column, which combines reversed-phase and anion-exchange mechanisms, the authors achieved stable retention of C2–C4 PFAS. Optimized pH control using ammonium hydroxide and acetic acid further stabilized retention times of highly polar compounds.

For mass spectrometric confirmation, the team demonstrated the use of the m/z 19 fragment transition as a new confirmatory ion for PFAS that previously lacked one. On the Xevo TQ Absolute system, low-mass transmission enhancement significantly increased sensitivity for this ion, allowing confirmatory detection of PFBA and PFPeA even at low (ppt-level) concentrations. Ion ratio stability across calibration curves met common method validation criteria (±30%), demonstrating robustness for routine use.

The combined method enables the simultaneous analysis of ultra-short to long-chain PFAS in a single injection without requiring additional columns or HRMS verification. Results from landfill leachate and surface water samples confirmed the method’s capability to resolve co-eluting interferences and to reliably identify PFAS at environmentally relevant levels. This workflow offers an efficient and practical solution for laboratories transitioning to include ultra-short chain PFAS within standard monitoring methods.