Automated mass spectrometric analysis of urinary free catecholamines using on-line solid phase extraction

Area of Science:

• Clinical Chemistry
• Analytical Chemistry
• Mass Spectrometry

Background:

• Catecholamine analysis in urine is crucial for diagnosing tumors.
• Current methods are complex, slow, and labor-intensive.

Purpose of the Study:

• Develop an automated on-line solid phase extraction method coupled to high performance liquid chromatography-tandem mass spectrometry (XLC-MS/MS).
• Quantify free catecholamines (epinephrine, norepinephrine, dopamine) in urine efficiently.

Main Methods:

• Automated on-line solid phase extraction using phenylboronic acid complexation.
• Reversed-phase chromatography with a pentafluorophenylpropyl column.
• Tandem mass spectrometry (MS/MS) with positive electrospray ionization in multiple reaction monitoring mode.

Main Results:

• Achieved a total run-time of 14 minutes.
• Demonstrated excellent linearity (R2>0.99) and low analytical variation (<10%).
• Established urinary reference intervals for epinephrine, norepinephrine, and dopamine in healthy subjects.

Conclusions:

• The developed XLC-MS/MS method offers high analytical performance, specificity, and sensitivity.
• This automated technique provides a more efficient and reliable approach for catecholamine quantification.
• The method is suitable for clinical diagnosis and treatment monitoring of catecholamine-producing tumors.