SC-CO₂ Extraction SOP — Nutmeg Oil

Perfect — here’s a COPI/CESI-ready SC-CO₂ Extraction SOP for Nutmeg (Myristica fragrans) Oil. This is designed for high-purity fractionation, maximizing key aroma compounds (sabinene, myristicin, elemicin, eugenol) for perfume-grade or therapeutic applications, while being compatible with industrial-scale SC-CO₂ systems.

1 — Raw Material Preparation

Material: Dried nutmeg seeds (10–12% moisture)

Steps:

  1. Inspect and sort seeds; remove damaged or moldy kernels.
  2. Grind to coarse powder (2–4 mm) to improve extraction efficiency while minimizing fines that could clog the system.
  3. Optional: Precondition with mild drying at 40°C to reach uniform moisture (max 10%).
  4. Store in airtight containers at cool, dark conditions until extraction.

Note: Avoid over-grinding; SC-CO₂ efficiency drops with powder <1 mm due to channeling.

2 — SC-CO₂ Extraction System Setup

Recommended System Parameters:

  • Extractor Vessel: 500–1000 mL pilot scale (adjust to industrial scale)
  • CO₂ Flow Rate: 15–25 kg/h per 100 kg nutmeg (adjust to system)
  • Pressure Range: 200–300 bar
  • Temperature Range: 35–45°C
  • Co-solvent (optional): Ethanol 5–10% to increase polar compound solubility

Rationale:

  • Low temperature preserves thermolabile monoterpenes.
  • Pressure range balances yield and selectivity.
  • Ethanol co-solvent increases yield of more polar components (e.g., myristicin).

3 — Loading and Sealing

  1. Load coarse nutmeg powder into extraction vessel.
  2. Ensure uniform packing to avoid channeling.
  3. Seal and leak-test vessel.

4 — Extraction Protocol

  1. Initial CO₂ flush: 5–10 min at low pressure to purge air.
  2. Pressurize to 200 bar, temperature 35°C, flow 15 kg/h CO₂.
  3. Stepwise pressure increase (optional): 200 → 250 → 300 bar to fractionate volatiles
  4. Extraction duration: 90–180 min depending on desired yield.
  5. Collect extract in separator(s) at controlled depressurization (50–70 bar) to avoid sudden flash-off of volatiles.

Notes:

  • Use multistage separators for fractionation (light top notes vs heavier aromatics).
  • Monitor pressure/temperature closely; record all system parameters for reproducibility.

5 — Post-Extraction Handling

  1. Recover SC-CO₂: recycle through compressor if system allows.
  2. Oil separation: decant or centrifuge to remove residual particulate.
  3. Storage: amber glass bottles, inert atmosphere (N₂), 15–20°C.
  4. Label: batch ID, date, fraction (top/middle/base notes).

6 — Fractionation Notes

  • Top fraction: high in sabinene, α-pinene, β-pinene — very volatile, citrusy-spicy notes
  • Middle fraction: myristicin, elemicin — warm, spicy, slightly sweet aroma
  • Base fraction: heavier sesquiterpenes, waxy notes — use in perfumery as fixatives

Tip: Separate fractions can be blended to create signature ANOC accords.

7 — Quality Control

  • GC-MS analysis: quantify major terpenes and phenylpropanoids
  • Sensory evaluation: aroma profile check against target chemotype
  • Moisture check: <0.1% residual water
  • Microbial screening: ensure extract is free from molds or bacteria

Target Specs:

  • Oil yield: 5–15% of seed dry weight
  • Key compounds: Sabinene 20–40%, Myristicin 5–10%, Elemicin 1–5% (varies with chemotype)

8 — Safety & Compliance

  • SC-CO₂ systems under high pressure → follow mechanical safety protocols
  • Co-solvent (ethanol) → ensure flammable material handling compliance
  • Waste nutmeg powder → compost or biofuel utilization
  • Maintain traceability for export/perfume-grade certification

9 — Scaling Considerations

  • Pilot scale: 500–1000 mL vessel → yields 50–100 g oil per run
  • Commercial scale: 50–500 L vessels
  • Continuous flow vs batch: Continuous SC-CO₂ preferred for large-volume production
  • Fractionation essential for high-value aroma compounds (perfume or therapeutic applications)

10 — Recordkeeping

  • Batch ID, seed origin, moisture content, grinding size
  • CO₂ pressure, temperature, flow rate, duration
  • Oil yield and fraction
  • GC-MS results and sensory notes

This ensures reproducibility for CESI operations and traceability for ANOC perfumery use.

If you want, I can now generate a matching step-by-step SC-CO₂ extraction SOP for Mace (aril) and essential oil fractionation, optimized for high-value perfume blends, including fractionation of top/middle/base notes for ANOC, fully ready for lab implementation.

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