Mass Spec Roundup: Early Life, Fullerenes, and Spiders…

Echoes from Earth’s Dawn

A new study in PNAS has uncovered chemical evidence of ancient life preserved in 3.3-billion-year-old rocks, pushing the detectable record of biomolecules back by more than a billion years. Using pyrolysis–gas chromatography–mass spectrometry (Py-GC-MS) combined with supervised machine learning, researchers from the Carnegie Institution for Science identified molecular patterns that reliably distinguish biological from non-biological material – even when original biomolecules have long since broken down.

The team analyzed 406 samples, from modern plants and animals to fungi, meteorites, synthetic organics, and Archean sediments. Their model separated biotic from abiotic sources with over 90% accuracy. “Our results show that ancient life leaves behind more than fossils; it leaves chemical ‘echoes.’ Using machine learning, we can now reliably interpret these echoes for the first time,” said Robert Hazen, corresponding author.

The approach also detected molecular signatures of oxygen-producing photosynthesis in 2.52-billion-year-old rocks, extending the chemical record of this metabolism by roughly 800 million years. By recognizing complex biochemical patterning rather than intact molecules, the method opens a new window onto Earth’s early biosphere and offers a promising framework for astrobiology. 

High-Temperature Pyrolysis Enables Giant Fullerene Growth

Researchers from Xiamen University have developed an ultra-high-temperature flash vacuum pyrolysis (UT-FVP) system capable of forming giant fullerenes – carbon cages larger than C₁₀₀ – from single-carbon molecules in just 15 seconds at ~3,000 °C. Described in CCS Chemistry, the method overcomes long-standing barriers in producing and isolating these low-yield, tightly bound carbon structures.

Because giant fullerenes adhere strongly to soot via π–π interactions, traditional ultrasonic or Soxhlet extraction fails to recover them. The researchers optimized two physical separation techniques, mechanical grinding and high-temperature sublimation, to free these cages from the soot matrix. Sublimation at up to 2,500 °C proved especially effective, yielding a smooth mass distribution centered near C₁₃₈ and extending beyond C₂₃₀ – the first macroscopic detection of such large fullerenes.

Using laser desorption/ionization TOF mass spectrometry (LDI-TOFMS), the team confirmed pristine carbon cages up to 2,760 Da, with characteristic 24 Da peak spacing indicating intact fullerene frameworks. The study also shows that both temperature and chlorine content steer fullerene growth: higher temperatures and more chlorinated precursors shift products toward larger cages.

Importantly, the separation workflow also recovers giant fullerenes previously undetected in soot from flame and arc-discharge methods, offering a broadly applicable strategy for fullerene research and enabling scalable access to these elusive carbon nanostructures. 

How Clubiona Combat the Cold

Clubiona spiders manufacture a unique class of antifreeze proteins (AFPs) that stop ice crystals from expanding inside their tissues, according to a new FEBS Journal study. Using mass spectrometry and structural modelling, scientists found that these AFPs form a previously unseen beta-solenoid fold, allowing the proteins to bind ice with remarkable efficiency.

Although the proteins resemble those found in beetles and moths, they evolved independently, making Clubiona AFPs a striking example of convergent evolution. The spiders’ antifreeze activity is exceptionally strong – more than 4 °C of thermal hysteresis – placing them among the most cold-hardy arthropods known.

Because Clubiona spiders remain active in orchards during winter, they continue feeding on pests such as pear psyllids at a time when most predators are dormant. “The ability of Clubiona and other winter-active spiders to continue to fend off pests in freezing temperatures is particularly important for perennial agriculture,” said corresponding author Peter Davies in a recent press release. “They could potentially be used to decrease reliance on insecticides, and therefore also combat insecticide resistance.”

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