Optimization of an enzymatic method for the determination of lysosomal N-acetyl-beta-D-hexosaminidase and beta-glucuronidase in synovial fluid

Clin Chem Lab Med. 2006;44(8):933-7. doi: 10.1515/CCLM.2006.177.

Abstract

Background: Our goal was to develop a suitably sensitive assay for N-acetyl-beta-D-hexosaminidase (HEX) and beta-glucuronidase to allow their use as markers of joint diseases.

Methods: We optimized a spectrophotometric method for the determination of lysosomally derived HEX and beta-glucuronidase in synovial fluid on a microplate reader to improve its utility. HEX and beta-glucuronidase act on the 4-nitrophenyl derivatives N-acetyl-beta-glucosamine and beta-D-glucuronide, respectively, to produce 4-nitrophenol, which can be measured at 405 nm on a microplate reader.

Results: Maximum enzyme activity was observed at pH 4.7 in a citrate-phosphate buffer for HEX and at pH 4.5 in an acetate buffer for beta-glucuronidase. A 10-microL sample with 30 microL of substrate solution and 40 microL of appropriate buffer produced measurable amounts of 4-nitrophenol after incubation for 60 min at 37 degrees Celsius. Reactions were terminated by the addition of 200 microL of 200 mM borate buffer (pH 9.8).

Conclusions: The assay is sufficiently sensitive for small volumes of synovial fluid, and is useful for the clinical diagnosis of joint diseases.

MeSH terms

  • Aged
  • Arthritis, Rheumatoid / enzymology*
  • Biomarkers / metabolism*
  • Female
  • Glucuronidase / metabolism*
  • Humans
  • Hydrogen-Ion Concentration
  • Lysosomes / enzymology*
  • Male
  • Middle Aged
  • Spectrophotometry / methods
  • Substrate Specificity
  • Synovial Fluid / enzymology*
  • beta-N-Acetylhexosaminidases / metabolism*

Substances

  • Biomarkers
  • Glucuronidase
  • beta-N-Acetylhexosaminidases