Millisecond cryo-trapping by the spitrobot crystal plunger simplifies time-resolved crystallography

Nat Commun. 2023 Apr 25;14(1):2365. doi: 10.1038/s41467-023-37834-w.

Abstract

We introduce the spitrobot, a protein crystal plunger, enabling reaction quenching via cryo-trapping with a time-resolution in the millisecond range. Protein crystals are mounted on canonical micromeshes on an electropneumatic piston, where the crystals are kept in a humidity and temperature-controlled environment, then reactions are initiated via the liquid application method (LAMA) and plunging into liquid nitrogen is initiated after an electronically set delay time to cryo-trap intermediate states. High-magnification images are automatically recorded before and after droplet deposition, prior to plunging. The SPINE-standard sample holder is directly plunged into a storage puck, enabling compatibility with high-throughput infrastructure. Here we demonstrate binding of glucose and 2,3-butanediol in microcrystals of xylose isomerase, and of avibactam and ampicillin in microcrystals of the extended spectrum beta-lactamase CTX-M-14. We also trap reaction intermediates and conformational changes in macroscopic crystals of tryptophan synthase to demonstrate that the spitrobot enables insight into catalytic events.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Crystallography / methods
  • Crystallography, X-Ray
  • Humidity
  • Proteins* / chemistry
  • Temperature

Substances

  • Proteins