Practical Solid Phase Extraction Workflows for LC–MS / GC–MS Sample Preparation

Solid Phase Extraction (SPE) is widely used across food safety, pharmaceutical QC and environmental monitoring, where complex sample matrices demand efficient cleanup and high recovery.

This article presents practical application notes summarizing optimized SPE workflows, sorbent selection and extraction strategies for the most common analytes in Pharmaceutical Analysis.

Application note provides:

• Recommended SPE sorbent(s)
• Typical workflow steps
• Key method considerations
• Matrix cleanup challenges and solutions

Impurities & Degradation Products

Recommended sorbents:

• C18 – standard for reversed-phase LC analysis
• SCX – for basic impurities
• MAX – for acidic impurities

Typical workflow:

1. Condition SPE cartridge
2. Load diluted formulation extract
3. Wash gently to remove excipients
4. Elute impurities of interest
5. Analyze via LC–MS/MS

Notes:

Select ion exchange sorbents when API/excipient interference is strong.

Drug Metabolites in Plasma/Serum

Recommended sorbents:

• HLB – excellent protein interference removal
• MCX – for basic metabolites
• C18 – for non-polar metabolites

Typical workflow:

1. Perform protein precipitation (ACN or MeOH)
2. Load supernatant onto SPE cartridge
3. Wash: water → 5–20% MeOH
4. Elute: MeOH/ACN with modifiers
5. Analyze via LC–MS/MS

Notes:

A combination of protein precipitation + SPE dramatically improves signal.

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