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 Food Safety Testing.

Application note provides:

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

Pesticide Residue Analysis (Fruits, Vegetables, Grains)

Recommended sorbents:

• PSA (Primary Secondary Amine) – removes sugars, fatty acids, organic acids
• GCB (Graphitized Carbon Black) – removes pigments and planar molecules
• C18 – reduces hydrophobic interferences

Typical SPE workflow:

1. Extract sample with acetonitrile (or QuEChERS extraction)
2. Load onto PSA or PSA/GCB SPE column
3. Wash: acetonitrile/water (varying ratios)
4. Elute analytes with ACN or MeOH
5. Direct injection to GC–MS/MS or LC–MS/MS

Notes:

• Excessive GCB can adsorb planar pesticides; adjust sorbent mass carefully.
• For high-chlorophyll samples (spinach), combine PSA + GCB + C18.

Mycotoxins in Nuts, Grains and Cereals

Recommended sorbents:

• HLB polymer – broad analyte coverage
• PSA – removes fatty acids and pigments

Typical workflow:

1. Extract with acidified methanol/water
2. Condition HLB with MeOH → Water
3. Load extract
4. Wash with water or 5% MeOH
5. Elute with MeOH or ACN
6. Evaporate & reconstitute for LC–MS/MS

Notes:

HLB offers excellent recovery for aflatoxins, ochratoxins, DON, ZEN.

Veterinary Drug Residues (Meat, Milk, Aquatic Products)

Recommended sorbents:

• MCX (mixed-mode cation exchanger) – excellent for basic drugs
• HLB – for wide chemical classes

Typical workflow:

1. Load extract onto MCX at low pH (protonated analytes bind strongly)
2. Wash: water → methanol
3. Elute: MeOH with ammonium hydroxide

Notes:

MCX provides superior selectivity for sulfonamides, fluoroquinolones, macrolides.

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