Pesticide remediation of mother liquor, lot OBX-ML-071426-007

Document no.

SOP-OBX-ML-071426-007-R0

Revision

R0, draft

Source COA

Encore Labs, 2607ENC0296_1017

COA method

SOP CA_M-PESTMYCOLCMS

COA tested

08/03/2026

Producer

MoloWorx, AL

Jurisdiction

Alabama (ADAI, ADEM)

Target

non-detect at the lab LOD

1. Purpose and scope

Remove the residues listed in section 2 from mother liquor lot OBX-ML-071426-007 to non-detect, retaining as much cannabinoid as the chemistry allows, and prove the removal by the checks in section 4. The material is viable product. Waste handling applies only to removed fractions and used adsorbent.

Absolute zero cannot be measured. "Removed" in this SOP means non-detect at the reporting lab's LOD, on a method shown to detect the analyte in the final product matrix.

2. Basis: what the COA found

Limits are those printed on the COA by a California lab for an Alabama producer. They are not Alabama limits. A result of <LOQ is treated as its LOQ for planning, and does not count as non-detect. This COA is for distillate; the mother liquor itself must be assayed to set the true baseline.

Lot-specific risks

• Over the limit: Myclobutanil (1.47× limit) and Hexythiazox (1.15× limit).
• No removal data found for Boscalid, Propiconazole and Piperonyl Butoxide. Behavior on the column is an assumption until Phase 0.
• Bifenthrin: May tail into later fractions because of strong sorption.
• Bifenazate: Fast hydrolysis: keep water out and the pH neutral.
• Permethrin: Melting point 34.5 C, so it can soften near a 35 to 40 C dissolve or dry step.
• Permethrin: Report both isomers.
• 8 analytes at once usually points to a source or input problem. Trace the biomass lot before spending on cleanup.

3. Definitions

• ND: result below the LOD on the COA. <LOQ: detected but not quantifiable, and not ND.
• Reduction factor: baseline µg/g ÷ final µg/g. If the final is ND, it is reported as at least baseline ÷ LOD.
• Pool: fractions combined as product. Shoulder: cannabinoid-rich fractions just outside the pool, held for a second pass.
• Closure: analyte mass recovered across all streams ÷ analyte mass loaded.

4. Acceptance criteria and verification

Removal is verified four ways. Each has a measurable criterion. Ranges marked proposed are my proposals from common analytical practice, not sourced standards, so set them in your validation policy.

4.1 Release criteria for the final product

4.2 Release results, per analyte

4.3 Mass balance, proof that the molecules went somewhere else

On Phase 0 and each validation batch, assay every fraction, the column strip (strong solvent wash of the used adsorbent) and the rinses. Enter analyte mass in µg (ng/mL × mL ÷ 1000). A closure far below 80% means the analyte was lost or degraded, and the removal claim fails.

4.4 Process validation and what it proves

• Run three consecutive validation batches on this lot type. Each must meet A1 to A8. proposed
• Three passes in a row prove repeatability on those three runs. They do not prove a pass rate: with zero failures in 3 runs, one can claim only 95% confidence that at least 37% of batches pass. Claiming 90% reliability needs 29 passing runs, and 95% needs 59.
• So release is by lot, not by process. Every production lot is tested to A1 to A3 and A6 before it leaves quarantine, until ADAI says otherwise.
• Any change to the adsorbent lot, solvent lot, loading, flow, feed matrix or column size reopens validation for that change.

4.5 Out of specification

• Any failed criterion puts the lot on hold and is logged as a deviation.
• Do not reblend the lot or rerun it without a written plan approved by the reviewer. A second pass is allowed only under a pre-approved protocol with its own mass balance.
• If the analyte appears in the pool, change the adsorbent lot and repeat Phase 0 before the next batch.

5. Retention of cannabinoids

Estimated first-pass recovery under the prior model is 16% (P10 to P90 0 to 72%). This is assumption-driven and is replaced by the Phase 0 optimizer result once fraction data exists.

• The pool is the widest cannabinoid block that meets every target, chosen from fraction data.
• Shoulder fractions are held and re-run. Activated carbon and distillation are not used as the fix.
• Record every fraction's cannabinoid mass. Pooled cut points:

6. Procedure

Process values to record after Phase 0: loading concentration adsorbent per g solids flow fraction volume

Phase 0: Bench validation for this lot

Nothing here is validated. This phase produces the numbers that replace every assumption on this page.

Phase 1: Pretreatment

Fill the orange values from Phase 0.

Phase 2: Column run and pool

The pool is chosen from data, not by a fixed rule.

Phase 3: Recover and crystallize

Treat every new mother liquor as untested.

Release: QC and acceptance

Only the lab result counts. Never release on an in-process number.

7. Records

• Batch record: mother liquor lot, source biomass lot, mass, volume, adsorbent type and lot, solvent lots, loading, flow, fraction volumes and results.
• Product mass, recovery, COA, second-lab report, waste manifests.
• Operator, reviewer, date and time for each phase, and every deviation.
• Retain a sealed sample of the mother liquor, the pool and the final product.

8. Waste and safety

• Segregate three streams: analyte-bearing fractions, used adsorbent and filters, and recovered solvent. Label each with contents, lot and date.
• Run the ADEM waste determination (Ala. Admin. Code r. 335-14-3-.01(2)) on the fractions and spent media before shipment. Waste codes were not checked for Myclobutanil, Hexythiazox, Bifenthrin, Bifenazate, Boscalid, Permethrin, Propiconazole and Piperonyl Butoxide. The solvent stream is ignitable (D001) if hexane or petroleum ether.
• Solvent handling follows your extraction-room controls. Use nitrile over laminate gloves, splash goggles, lab coat and a fume hood. General practice, not from a source.

9. Open regulatory items

• Alabama limit for each analyte above, and whether sale of remediated material from a contaminated lot is allowed.
• Which labs ADAI accepts for release testing, and whether your ADAI license covers this step.
• Which agency governs finished CBD products. One secondary source names the ABC Board under HB 445, so verify against the statute.
• Your ADEM generator category and any notification duty.

10. Approval

11. References

• EPA SW-846 Method 3620C, Florisil cleanup
• Biotage, myclobutanil removal from cannabis oil
• J Cannabis Research, pesticide remediation strategy for preparative LC
• PPDB myclobutanil, permethrin, bifenazate
• NPIC malathion
• Ala. Admin. Code ch. 80-10-21 (ADAI hemp), ADEM hazardous waste determination