A Study of Filter Types Used in Sample Preparation of Cannabis/Hemp with HPLC Analysis

Applications | 2019 | ShimadzuInstrumentation
Sample Preparation, HPLC
Industries
Food & Agriculture
Manufacturer
Shimadzu

Summary

Importance of Topic


Reliable analysis of cannabinoids in cannabis and hemp is crucial for quality control, regulatory compliance and product development. Filtration during sample preparation eliminates particulates for high-performance liquid chromatography (HPLC), but adsorption to syringe filters can reduce analyte recovery. This study examines filter-material effects on phytocannabinoid recovery to optimize potency testing workflows.

Objectives and Study Overview


The primary goal was to compare recovery rates of 11 key phytocannabinoids following filtration through seven syringe filter materials using a standardized HPLC method. A secondary objective was to assess whether filter hydrophilicity or hydrophobicity correlates with analyte loss. Seven filter types were evaluated without pre-wetting: hydrophobic PVDF, hydrophilic PVDF, polypropylene (PP), PTFE, nylon, cellulose acetate (CA) and polyethersulfone (PES).

Methodology


Solvent spiking and unspiked controls were prepared in methanol containing a certified 11-component phytocannabinoid mix. Calibration curves spanned 0.5–100 μg/mL across 11 cannabinoids, achieving r2 ≥ 0.9992. Quality control (QC) samples at 20 and 80 ppm evaluated accuracy and precision before and after each filter test. Filtration replicates (n=10 per filter type) were analyzed using gradient HPLC with UV detection.

Instrumentation Used


  • Shimadzu Cannabis Analyzer for Potency™ integrated HPLC with UV detector at 220 nm
  • Column: NexLeaf CBX for Potency, 2.7 μm, 4.6×150 mm with guard cartridge
  • Mobile phases: 0.085% phosphoric acid in water (A) and acetonitrile (B)
  • Gradient: 70%–95% B over 8 min, total run ~11 min
  • Flow rate: 1.6 mL/min; injection volume: 5 μL; oven: 35 °C
  • Syringe filters: 0.45 μm, 13 mm discs in various materials

Main Results and Discussion


Calibration exhibited excellent linearity (average r2 = 0.9996) and QC recoveries within ±2.6% accuracy. Unfiltered spiked solvent recoveries averaged 9.94 ppm (±0.63% RSD), confirming stability. Filtration efficiency revealed nylon and PTFE filters provided the lowest analyte loss (average recoveries ~9.7–10.2 ppm, RSD ≤ 0.9%). Hydrophilic and hydrophobic PVDF, PES and CA/PP filters showed greater variability (RSD up to 2.7%), but no consistent trend linked material hydrophobicity to retention.

Benefits and Practical Applications


  • Selecting nylon or PTFE syringe filters ensures robust phytocannabinoid recovery and reproducible results in potency assays
  • Minimizes sample loss and filter-related bias, critical for compliance and comparative studies
  • Standardized filtration protocols enhance method transferability across laboratories

Future Trends and Applications


Emerging filter technologies with tailored surface chemistries may further reduce analyte adsorption. Integration of inline filtration modules in automated platforms could improve throughput. Expanded evaluation of novel materials and micro- or ultrafiltration approaches will support high-throughput potency testing and impurity profiling.

Conclusion


This study demonstrates that filter material significantly influences phytocannabinoid recovery in HPLC sample preparation. Nylon and PTFE syringe filters delivered superior precision and minimal analyte loss, whereas other materials showed higher variability. These findings guide filter selection for accurate cannabis/hemp potency analysis.

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