Automation of solid-phase microextraction in high-throughput format and applications to drug analysis

Area of Science:

• Analytical Chemistry
• Forensic Toxicology
• Biomedical Analysis

Background:

• Traditional sample preparation methods for drug analysis are often time-consuming and labor-intensive.
• Automation is crucial for increasing laboratory throughput and reducing human error in bioanalytical methods.

Purpose of the Study:

• To develop and validate an automated solid-phase microextraction (SPME) method coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) for high-throughput drug analysis.
• To demonstrate the advantages of automated SPME over automated solid-phase extraction (SPE) for processing biological samples.

Main Methods:

• Automation of SPME using a 96 multiwell plate format, a multifiber device, orbital shakers, and a robotic system.
• Optimization of SPME parameters including coating selection, fiber coating, agitation uniformity, and calibration.
• Validation of the method for the analysis of diazepam, lorazepam, nordiazepam, and oxazepam in human whole blood using LC-MS/MS.

Main Results:

• The automated SPME-LC-MS/MS system processed 96 samples in 100 minutes, achieving the highest throughput for SPME to date.
• The method demonstrated excellent accuracy (87-113%), precision (
• Automated SPME offers lower cost, quantitative determination of free and total drug concentrations, and direct processing of whole blood without pretreatment compared to automated SPE.

Conclusions:

• The developed automated multifiber SPME-LC-MS/MS method is highly efficient and suitable for high-throughput analysis of drugs in human whole blood.
• Automated SPME presents significant advantages in terms of speed, cost-effectiveness, and sample handling flexibility for bioanalytical applications.