Automated In-Line SPE/HPLC/MS/MS
Wed 8:30 AM - Track 1: Sample Preparation Strategies
Kim Gamble
Kim Gamble, Microliter
Ken Lewis, OpAns
OpAns is a contract research company with a history of providing regulated (GLP) and non-regulated analytical services to support pharmaceutical research and development. Recently, OpAns expanded its product offering to include regulated (CLIA) clinical diagnostic assays. The result is a diversified customer base where all desire rapid turnaround on relatively small sets of samples (tens to hundreds).

This presentation describes our implementation of an automated, easy-to–use system for performing a variety of assays within one day on a single instrument system. Although the system is not ultra high-throughput (200 to 300 samples per day), the automation and flexibility has increased our efficiency and productivity on multiple MS/MS instrument platforms (Agilent, Thermo) for a variety of analytes (e.g., Drugs of Abuse, Steroids, Vitamins).

The solution described in this presentation contains the following components:

  • A standard CTC PAL autosampler coupled to an HPLC pump and triple quadrupole mass spectrometer; all are controlled using the mass spectrometer’s software (e.g., MassHunter, Xcaliber)
  • ITSP SPE devices and tray from MicroLiter Analytical Supplies, Inc.

These components support the following workflow:

  1. Minimal sample preparation, such as

    • Centrifigation of urine and serum/plasma matrices to remove particles/clots
    • Precipitation of proteins from whole blood matrices
    • Stabilization of the analytes in the sample matrix.

  2. The samples are transferred into vials or 96-well plates.
  3. The PAL is loaded with samples, ITSP devices, and solvents.
  4. A sample queue is created in the mass spectrometer’s control software.
  5. As each sample is analyzed on the MS/MS syytem, the next sample is being prepared by the PAL.
  6. The data is processed post-run and the results reported.