U.S. Patent US12559784B2WIPO WO2024177860A1NIH/NIEHS R44 ES036065

In Chemico Test for Toxicity — U.S. Patent US12559784B2

A cell-free, enzyme-activity-based platform that measures biochemical impact across nine human tissue compartments simultaneously. No animals. No cell culture. GHS-compliant results in 6 hours.

Granted: February 24, 2026
Inventors: Stewart Lebrun PhD & Linda Nguyen
Assignee: Lebrun Labs LLC
NIH Support: NIH/NIEHS SBIR Fast-Track R44 ES036065
What the Patent Covers

What the Patent Covers

The invention describes a cell-free, reagent-based assay in which a test material is exposed to a defined enzyme or enzyme mixture. The degree to which the test material reduces enzymatic activity is used to predict the extent and classification of toxicity to living tissue. Because the assay uses no animal tissues, cells, or cell cultures, it is classified as an in chemico method — the most shelf-stable and field-deployable category of nonanimal test under OECD guidelines.

Shelf-stable reagent kit format suitable for field use and high-throughput laboratory screening, applicable to acids, alkalis, oxidizers, and surfactants.

Core Method Claims
1

Applying a test substance to a predefined enzyme or enzyme mixture to effect an in chemico reaction

2

Measuring any reduction in enzymatic activity on a predefined substrate

3

Comparing the measured reduction to a control or previously established activity value

4

Predicting the extent or classification of living tissue toxicity based on the measured reduction

International Patent Protection
PCT Application PCT/US2024/015781, published as WO2024177860A1 on August 29, 2024. Designates all PCT member states — patent protection pathway in 150+ countries.
Broad Tissue Applicability

Nine Human Tissue Compartments

The enzyme-activity reduction platform is not limited to skin. The WIPO abstract and patent specification disclose applicability to the full spectrum of human tissue toxicity assessment.

Skin (Dermal)

DermaSafe SCT (ICSC)

The most developed application, commercialized as DermaSafe SCT (In Chemico Skin Corrosion Test). Resolves GHS Category 1 into subcategories 1A, 1B, and 1C — a key differentiator over RhE models which typically resolve only Category 1 as a whole. Correlates quantitatively with depth of injury for DOT packing group assignment.

Enzyme:Biomimetic skin enzyme substrate
GHS output:GHS Cat. 1A / 1B / 1C · Not Corrosive
Regulatory:OECD TG 431, DOT 49 CFR Part 173

Ocular (Eye)

Complements IVD EIT (OptiSafe)

The enzyme-activity reduction principle extends directly to ocular toxicity prediction. The eye contains lysozyme, lactate dehydrogenase, and corneal esterases that can be modeled in an in chemico format. Provides a pathway to a fully cell-free ocular irritation test complementing the OECD TG 496-listed OptiSafe platform.

Enzyme:Corneal esterase / lysozyme
GHS output:GHS Cat. 1 Serious Eye Damage · Cat. 2 Eye Irritation · Not Classified
Regulatory:OECD TG 492, OECD TG 496

Pulmonary (Lung)

Industrial chemical, aerosol, pharmaceutical inhalation

The lung presents surfactant-associated proteins, proteases, and oxidoreductases that can be modeled using the enzyme-activity reduction platform. Applications include assessment of aerosols, vapors, and respirable particulates for occupational and consumer safety.

Enzyme:Surfactant protein / lung esterase
GHS output:Acute Inhalation Hazard Cat. 1–3
Regulatory:OECD TG 403, REACH inhalation hazard

Hepatic (Liver)

Drug candidate screening, DILI prediction

The liver is the primary site of xenobiotic metabolism. Liver-specific enzymes including ALT, AST, and CYP450 isoforms are well-characterized biomarkers of hepatotoxicity. The platform can be configured with hepatic enzyme panels to provide a rapid, cell-free screen for hepatotoxic potential before IND-enabling studies.

Enzyme:ALT / AST / CYP450 isoforms (CYP3A4, CYP2D6, CYP1A2)
GHS output:STOT-RE Cat. 1/2 (DILI)
Regulatory:ICH S2(R1), OECD TG 471–490, FDA DILI guidance

Neurological

Pesticide safety, CNS drug screening, solvent classification

The nervous system relies on tightly regulated enzymatic processes including acetylcholinesterase (AChE) — the target of organophosphate and carbamate pesticides. AChE inhibition is a validated endpoint for predicting cholinergic toxicity. The A/B ratio (AChE vs BChE inhibition) distinguishes true cholinesterase inhibitors from non-selective inhibitors.

Enzyme:Acetylcholinesterase (AChE) / BChE / MAO / NSE
GHS output:STOT-SE Cat. 1 (Neurotoxic)
Regulatory:OECD TG 424, EPA neurotoxicity, REACH CMR

Developmental / Reproductive

Pharmaceutical teratogenicity, endocrine disruptor ID, cosmetic safety

Key enzymatic processes involved in retinoic acid signaling, folate metabolism, and steroidogenesis can be disrupted by toxic chemicals. CYP19A1 (aromatase) inhibition is a primary endpoint for endocrine disruptor identification under EPA EDSP screening.

Enzyme:RALDH / DHFR / Aromatase (CYP19A1) / steroidogenic enzymes
GHS output:Repr. 1A/1B/2 · Endocrine disruptor
Regulatory:OECD TG 414, REACH Repr., ICH S5(R3), EPA EDSP

Acute Systemic

Industrial GHS classification, pharmaceutical safety, emergency response

The platform can be configured as a broad-spectrum acute toxicity screen using panels of enzymes representative of multiple organ systems, providing a rapid tier-1 assessment before more targeted tissue-specific testing.

Enzyme:Multi-enzyme panels: hepatic, renal, cardiac, hematological markers
GHS output:GHS Acute Tox. Cat. 1–5
Regulatory:OECD TG 129, GHS acute toxicity, REACH acute assessment

Renal (Kidney)

Heavy metal safety, antibiotic nephrotoxicity, contrast agent safety

The kidney is a major target of chemical toxicity due to its role in concentrating and excreting xenobiotics. Renal tubular enzymes including NAG, alkaline phosphatase, and GGT are sensitive biomarkers of nephrotoxicity. The platform can predict renal tubular injury from industrial chemicals, heavy metals, and pharmaceutical compounds.

Enzyme:NAG / GGT / alkaline phosphatase / KIM-1 associated enzymes
GHS output:STOT-RE Cat. 1/2 (Nephrotoxic)
Regulatory:OECD TG 407/408, ICH S7A, REACH renal toxicity

Cardiac

Pharmaceutical cardiovascular safety, industrial cardiac hazard

Cardiotoxicity is a leading cause of drug withdrawal from the market. Cardiac-specific enzymes including CK-MB and LDH-1 isoforms can be incorporated into the platform to provide a rapid, cell-free screen for chemicals with cardiotoxic potential.

Enzyme:CK-MB / LDH-1 isoforms / cardiac phosphodiesterases
GHS output:STOT-SE Cat. 1/2 (Cardiotoxic)
Regulatory:ICH S7B, FDA cardiac safety, OECD cardiovascular guidelines
High-Throughput Method

High-Throughput Workflow: Chemical to Report in 6 Hours

Using standard 96-well or 384-well microplate formats, automated liquid handling, and a high-throughput spectrophotometric plate reader, a single operator can test up to 30 different chemicals simultaneously across the full human tissue panel.

30 chemicals simultaneously
Throughput
6 hours sample to report
Turnaround
96-well or 384-well microplate
Format
1

Sample Intake

Up to 30 test materials (industrial chemicals, drug candidates, consumer product formulations, or environmental samples) are received and logged. Each material is prepared at a defined concentration range in aqueous buffer.

2

Automated Plate Setup

An automated liquid handling robot aspirates and dispenses test materials, enzyme reagents, and substrate solutions into the microplate wells. Each well receives a precisely metered volume (10–50 µL per well in 384-well format), enabling all 30 test chemicals to be run in triplicate across the full tissue enzyme panel on a single plate.

3

Incubation: Enzyme-Chemical Reaction

Plates are incubated at 37°C for a defined period (typically 1–4 hours depending on the tissue enzyme panel). The test chemical reacts with the enzyme reagent. Chemicals toxic to a given tissue type reduce the activity of the corresponding enzyme — the greater the toxicity, the greater the reduction.

4

Spectrophotometric Plate Reader

After incubation, the substrate solution is added and the plate is read by a high-throughput spectrophotometric plate reader (e.g., BioTek Synergy Neo2, Molecular Devices SpectraMax). Reduced absorbance relative to the enzyme-only control indicates enzyme inhibition and predicted tissue toxicity. A full 384-well plate is read in under 2 minutes.

5

384-Well Microplate Format

The 384-well format enables all 30 test chemicals to be run in triplicate across 9 tissue enzyme panels on a single plate, with sufficient wells remaining for positive and negative controls. Low reaction volumes (10–50 µL per well) minimize reagent consumption and allow testing of precious or limited-quantity samples.

6

Report Generation

Raw absorbance data are processed to calculate percent enzyme activity remaining for each test chemical × tissue panel combination. Results are expressed as a quantitative toxicity score and a GHS/regulatory classification. A complete multi-tissue toxicity report for all 30 chemicals is generated within 6 hours of sample receipt.

Total elapsed time
≤ 6 hours from sample receipt to final report
Up to 30 chemicals tested simultaneously
~30 min
Sample intake
~45 min
Plate setup
1–4 hrs
Incubation
~30 min
Read + analysis
~30 min
Report
Example Report Output

Full Human Tissue Panel Report

Example output for a strong oxidizing agent (10% NaOCl, CASRN 7681-52-9) tested across all nine tissue enzyme panels. Up to 30 test chemicals in a batch receive an equivalent multi-tissue profile within the same 6-hour run.

ICSC REPORT OUTPUT · LEBRUN LABS LLC · v2.4.1
SODIUM HYPOCHLORITE, 10% w/v
CASRN: 7681-52-9 · MW: 74.44 g/mol · Formula: NaOCl
Report ID: RPT-2024-0047
Run time: 5h 52m
Status: COMPLETE
Tissue PanelEnzyme MarkerWells% Act. RemainingClassification
Skin (Dermal)Biomimetic skin enzyme substrateA1–A34.2%GHS Cat. 1A: Corrosive (DOT PG I)
Ocular (Eye)Corneal esterase / lysozymeB1–B37.1%GHS Cat. 1: Serious Eye Damage
Pulmonary (Lung)Surfactant protein / lung esteraseC1–C311.3%Acute Inhalation Hazard: Cat. 1
Hepatic (Liver)ALT / CYP3A4 activityD1–D338.4%Moderate hepatotoxic potential
NeurologicalAcetylcholinesterase (AChE)E1–E382.1%Not classified, low neurotoxic potential
Developmental / Repro.RALDH / aromatase (CYP19A1)F1–F344.0%Potential endocrine disruptor, flag
Acute SystemicMulti-organ enzyme panelG1–G39.0%GHS Acute Tox. Cat. 1: Oral/Dermal
Renal (Kidney)NAG / GGT activityH1–H351.2%Moderate nephrotoxic potential
CardiacCK-MB / LDH-1 isoformsI1–I376.3%Not classified, low cardiotoxic potential
CTRL WELLS P1–P6 · VEHICLE: PBS pH 7.4 · MEAN CTRL ACT: 100.0% ± 2.3%
Use Cases

Applications of the Full Human Tissue Panel

Drug Development

Screen 30 structural analogs simultaneously to identify the candidate with the most favorable multi-tissue safety profile. Hepatic enzyme panel results (ALT, CYP3A4) flag DILI potential before IND-enabling studies. CK-MB and LDH-1 isoform data provide early cardiotoxicity signals complementing hERG channel assays.

ICH S2(R1)ICH S7ADILI predictionLead optimization

Regulatory Toxicology

Multi-tissue results directly support GHS hazard classification across multiple endpoints from a single test run. Supports REACH registration, OECD test guideline submissions, DOT packing group assignment, and FDA cosmetic/OTC drug safety substantiation under MoCRA.

GHS classificationREACHOECDDOTMoCRA

Research Toxicology

Rapidly map the toxicological SAR of a chemical series across nine tissue types. Test complex mixtures for multi-tissue hazard in a single run. Use tissue-specific enzyme inhibition patterns to generate mechanistic hypotheses. Compatible with HTS workflows for large compound library screening.

SAR studiesMixture toxicologyHTSMechanism of action

Industrial Chemical Safety

Provides a cost-effective alternative to in vivo studies for REACH Annex VII–X endpoints. Dermal and systemic toxicity data support DOT packing group assignment and proper shipping name determination for hazardous materials transport.

REACH Annex VII–XDOT hazmatGHS SDSTSCA
AI-Driven Analysis

AI-Driven Analysis of Multi-Tissue OD Data

The nine-tissue OD matrix is a high-dimensional dataset ideally suited for machine learning. AI analysis produces predictions of human toxicity that are more accurate, more mechanistically informative, and more directly applicable to human risk assessment than any existing approach.

Supervised GHS Classification

Gradient-boosted tree models (XGBoost) or random forests trained on reference datasets predict GHS hazard categories directly from the OD matrix. Published benchmarks for single-tissue in chemico assays achieve 85–92% concordance with in vivo GHS classifications; the nine-tissue panel substantially exceeds this by providing cross-tissue context.

Deep Learning for Mechanism-of-Action

A CNN or transformer architecture trained on the full OD matrix, treating the 9 × N concentration-response matrix as an image, learns to classify compounds by mechanism of action without explicit feature engineering — covering membrane disruption, reactive metabolite formation, cholinesterase inhibition, endocrine disruption, and mitochondrial toxicity.

QSAR Integration

The OD matrix combined with molecular descriptors (RDKit, Mordred) trains multi-output QSAR models that predict tissue-specific toxicity from chemical structure alone. A multi-output neural network with nine output nodes enables virtual screening of large compound libraries for multi-tissue hazard before any physical synthesis.

PBPK Model Integration

Tissue-specific EC₅₀ values from the OD matrix are directly usable as input parameters for physiologically based pharmacokinetic (PBPK) models. Coupling in chemico data with PBPK enables prediction of target tissue concentration, margin of exposure, route-of-exposure sensitivity, and sensitive subpopulation risk.

Bayesian Uncertainty Quantification

Bayesian network models propagate uncertainty from raw OD measurements through dose-response fitting into the final GHS classification, producing a probability distribution over hazard categories. A submission reporting '95% probability of GHS Category 1 skin corrosion' is more informative and defensible than a point prediction.

Transfer Learning & Cross-Species Extrapolation

Pre-trained toxicology models (EPA ToxCast: 9,000+ chemicals, 700+ assays; NIH Tox21: 12,000+ chemicals, 72 assays) can be fine-tuned on the nine-tissue OD matrix using transfer learning. Fine-tuning on 200–500 compounds produces highly accurate predictions and enables cross-species extrapolation for regulatory submissions.

Roadmap

Development Outlook

Five-Year Outlook (2026–2031)

1
2026–2027
First commercial ICSC automated workstation prototype

Benchtop unit integrating robotic liquid handling, nine-tissue reagent dispensing, microplate reader, and AI analysis software. Validated against the reference dataset from NIH/NIEHS R44 ES036065. Target: 50 compounds/week, full GHS report in 6 hours.

2
2027–2028
OECD test guideline submission for the nine-tissue panel

Submission of a prevalidation dossier to the OECD Test Guidelines Programme, building on OECD TG 431 and TG 496 precedents. Parallel submission to EPA under the Alternative Test Method (ATM) program. Estimated timeline to OECD acceptance: 3–5 years from submission.

3
2028–2029
AI model release and open-science data contribution

Release of the first public nine-tissue QSAR model, trained on 500+ compounds. Contribution of the reference dataset to EPA DSSTox and NIH Tox21 databases. First peer-reviewed publications on AI-driven multi-tissue prediction accuracy versus in vivo outcomes.

4
2029–2031
Pharmaceutical and industrial adoption at scale

Integration into pharmaceutical lead optimization workflows at 10+ major pharma companies. Adoption by chemical manufacturers for REACH registration support. First regulatory submissions (EPA, ECHA) citing nine-tissue in chemico data as primary evidence for multi-endpoint GHS classification.

Twenty-Year Vision (2026–2046)

1
2031–2036
Global regulatory harmonization around in chemico multi-tissue data

OECD acceptance of the nine-tissue panel as a validated test method. EPA, ECHA, and FDA issue guidance recognizing multi-tissue in chemico data packages as sufficient for multi-endpoint GHS classification. Estimated impact: elimination of 500,000+ animal tests per year globally.

2
2033–2038
Personalized chemical safety assessment

Integration with human genomic databases enables prediction of individual-level chemical sensitivity based on genetic variants in metabolic enzymes (CYP2D6, CYP2C19, NAT2). The nine-tissue PBPK model, parameterized with individual genomic data, predicts personalized occupational exposure limits.

3
2036–2041
Real-time environmental and consumer product hazard monitoring

Miniaturized, field-deployable versions integrated into smartphones, wearable sensors, and environmental monitoring networks provide real-time chemical hazard assessment for drinking water, air quality, food safety, and consumer product safety.

4
2041–2046
AI-designed safe-by-construction chemicals

Accumulated nine-tissue OD profiles for hundreds of thousands of compounds, combined with molecular generative AI, enables design of new chemicals optimized simultaneously for desired function and minimal multi-tissue toxicity — making 'safe by construction' the default paradigm for new chemical development.

Available Now

Test Kits Based on This Technology

The patented enzyme-activity reduction platform is commercially available as validated test kits through InChemico — a wholly owned subsidiary of Lebrun Labs.

OECD TG 496

OptiSafe EIT™ Main Assay

SCU #OSMA2796$1,800 / kit
GHS output: GHS NC / Cat 2 / Cat 1
  • 100% sensitivity — zero false negatives for nonirritants
  • GHS NC or refers for further testing
  • No aseptic technique required
  • Shelf-stable vegan matrix
  • Results in under 24 hours
  • Kit tests 3 samples
Full GHS NC → Cat 1

IVD EIT™ Main Kit

SCU #IVDM3544$1,200 / kit
GHS output: GHS NC / 2B / 2A / Cat 1
  • Discriminates all 4 GHS eye categories (NC, 2B, 2A, 1)
  • >90% accuracy per GHS classification
  • Highest mechanistic relevance for ocular drug studies
  • Uses food-source animal eyes — qualifies as nonanimal
  • Only method to correctly discriminate GHS 2B vs. 2A
  • Requires IVD Viability or TUNEL kit (sold separately)
In Chemico · Patent US12559784B2

DermaSafe SCT™ High-Throughput

SKU #DSHT2903$1,800 / kit
GHS output: GHS 1A / 1B+1C / Not Corrosive
  • GHS 1A / 1B+1C / Not Corrosive classification
  • DOT packing group assignment (I, II+III, IV)
  • Colorimetric plate reader, high-throughput format
  • Results in under 6 hours at room temperature
  • Shelf-stable, no animals, no cell culture
  • Lab and field-deployable formats available
Prefer contract testing?

Submit samples directly to the Lebrun Labs affiliate lab for GHS classification reports and regulatory data packages. OptiSafe EIT™, IVD EIT™, and DermaSafe SCT™ testing available.

Cosmetics & Personal Care Industry

Eye Irritation & Skin Corrosion Testing for Cosmetic Manufacturers

The patented in chemico platform underpins OptiSafe (eye irritation test, OECD TG 496) and DermaSafe SCT (skin corrosion test) — validated nonanimal methods used by cosmetic manufacturers, ingredient suppliers, and CROs for GHS safety classification and regulatory labeling compliance.

Cosmetic Eye Irritation Testing (OECD TG 496)

OptiSafe is the only fully cell-free, in chemico eye irritation test listed in OECD Test Guideline 496. Cosmetic manufacturers use it to classify finished formulations, rinse-off products, eye-area products, and raw ingredients for GHS eye irritation hazard — without animal testing. Results in under 24 hours.

Eye irritation test cosmeticsOECD TG 496GHS Category 1 / 2 / NCNonanimalDraize alternative

Cosmetic Skin Corrosion Testing

DermaSafe SCT classifies cosmetic ingredients and formulations for GHS skin corrosion hazard (1A, 1B+1C, Not Corrosive) and DOT packing groups. 98% global accuracy — the highest of any validated method. Shelf-stable, high-throughput, no cell culture, no animals.

Skin corrosion test cosmeticsGHS 1A / 1B+1CDOT packing groupIn chemicoHigh-throughput

Cosmetic Ingredient Safety Screening

Screen new cosmetic ingredients — surfactants, preservatives, actives, fragrances — for ocular and dermal safety before formulation. The high-throughput platform tests up to 30 chemicals per run in under 6 hours across 9 human tissue types simultaneously.

Ingredient safety testingCosmetic ingredient screeningHigh-throughput9 tissue typesFormulation safety

GHS Regulatory Compliance & Labeling

Both OptiSafe and DermaSafe SCT generate GHS classification data accepted for regulatory submissions under REACH, GHS, and DOT. OptiSafe is listed in OECD TG 496 — the international standard for nonanimal eye irritation testing. Full regulatory data packages available from LebrunLabs.com.

GHS labeling cosmeticsREACH complianceRegulatory data packageOECD acceptedDOT classification
Cosmetic & Chemical Industry

Need eye irritation or skin corrosion testing for your cosmetic formulation?

OptiSafe (OECD TG 496) and DermaSafe SCT are available as test kits at InChemico.com or as contract testing services at LebrunLabs.com.

Patent & IP Details

U.S. PatentUS12559784B2
WIPO PublicationWO2024177860A1
PCT ApplicationPCT/US2024/015781
GrantedFebruary 24, 2026
Priority DateFebruary 24, 2023
Filing DateFebruary 14, 2024
WIPO PublishedAugust 29, 2024
InventorsStewart Lebrun PhD, Linda Nguyen
AssigneeLebrun Labs LLC
NIH SupportNIH/NIEHS SBIR Fast-Track Grant R44 ES036065
Contract Research & Licensing

Contract Research & Licensing

Lebrun Labs offers contract research services and licensing opportunities built on the patented enzyme-activity reduction platform. Whether you need GHS-compliant toxicity testing for a single chemical or are interested in licensing the technology for your own testing program, our team can help.

Research supported by NIH/NIEHS under Award Number R44 ES036065. Content does not represent official NIH views.

Lebrun Labs
Eye & Skin Research

Developer of the OptiSafe eye irritation test and DermaSafe SCT skin corrosion test — validated new approach methodologies (NAMs) for GHS classification. NIH/NIEHS SBIR funded.

Anaheim, CA · lebrunlabs.net

Contact

Lebrun Labs LLC3301 E. Miraloma Ave., Suite 194Anaheim, CA 92806(714) 345-4689[email protected]

Lebrun Labs LLC develops and validates new approach methodologies (NAMs) for chemical safety testing. The OptiSafe eye irritation test (IVD EIT, OECD TG 496 listed, NIH/NIEHS funded: R43ES025501, R44ES025501, R44ES031881, SB1 ES025501, SB1 ES038803) classifies GHS ocular hazard categories without animal tissue or cell culture. The DermaSafe SCT skin corrosion test (NIH/NIEHS SBIR R44ES036065) classifies GHS skin corrosion categories and DOT packing groups using an in chemico, cell-free spectrophotometric method. Both methods are supported by eight peer-reviewed publications in Toxicology In Vitro and Cutaneous and Ocular Toxicology, five U.S. patents, and 11 NIH grants awarded since 2015.

Research supported by the National Institute of Environmental Health Sciences under Awards R44ES031881, SB1 ES025501, SB1 ES038803 (OptiSafe eye irritation test) and R44ES036065 (DermaSafe SCT skin corrosion test), and by the National Eye Institute under Award R21 EY033713. Content does not represent official NIH views. Testing services provided through LebrunLabs.com.

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