# Electrochemically-Controlled Rapid Chromatographic Separation of Nuisance Compounds from Natural Product Extracts

> **NIH NIH R44** · MILLENNIAL MATERIALS AND DEVICES, INC. · 2022 · $518,112

## Abstract

Abstract
Natural products remain a rich source of compounds for drug discovery. However, a significant challenge for
high throughput bioassay screening against molecular targets is the isolation of bioactive compound mixture
free from interfering nuisance compounds. The well-established ubiquitous nuisance compounds in plant
extracts are Tannins - polyphenolic plant metabolites. The solid-phase extraction (SPE) process is now gaining
recognition as a method for rapid fractionation of crude plant extracts and employed to remove nuisance
compounds as well as purify and concentrate analytes before introducing them into more expensive gas- or
liquid- chromatography instrumentation. Our customer discovery interviews found that the challenges with
current reverse phase materials in the removal of nuisance compounds during natural product extraction
include unsuitable for more than single-use, pH (degrades at basic pH) and temperature (degrades at T >
60°C) restrictions, and suboptimal performance in the removal of nuisance compounds such as tannins. These
technical issues affected (increased) the operational costs to manufacture the product and decreased margins.
This SBIR Phase II proposal’s overall objective is to finalize an innovative solid phase extraction unit that
incorporates electrically-conducting all-carbon spherical microparticles (40 µM diameter), synthesized using
multi-walled carbon nanotubes (MWCNTs) as starting material. This material will, under an applied voltage,
facilitate selective separation and detection of tannins. During Phase II, two aims will be pursued. Aim 1.
Demonstrate that the all-carbon microbead synthesis and solid-phase extraction substrates are scalable. Aim
2. Establish consistent performance across the scaled-up microbead and substrate batches, and demonstrate
(a) improved retention of tannins, (b) rapid detection of trapped tannins by electrospray mass spectrometry,
and (c) reuse of the cartridge.
Expected outcomes include 1) Finalization of the setup and conditions that will enable the large scale
manufacturing of all-carbon solid-phase extraction system. 2) Identification of the critical synthesis process
parameters (CPP) that affects tannin extraction performance reproducibility and has to be monitored and
controlled to ensure the process produces the desired quality without batch variability. 3) Finalization of
scientifically sound and appropriate test methods that can eventually be qualified/validated for batch release
testing. The scientific outcomes from the Phase II activities will facilitate the commercial launch of this product
as well as enable its application for the removal of other nuisance compounds. Upon complete development,
NanoPak-C will attract customers seeking next-generation performance capabilities that fall outside the
capabilities of current state-of-art for the removal of nuisance compounds during natural product extraction and
advance separation of active drug candidates from the purif...

## Key facts

- **NIH application ID:** 10483473
- **Project number:** 1R44AT012008-01
- **Recipient organization:** MILLENNIAL MATERIALS AND DEVICES, INC.
- **Principal Investigator:** Balaji Sitharaman
- **Activity code:** R44 (R01, R21, SBIR, etc.)
- **Funding institute:** NIH
- **Fiscal year:** 2022
- **Award amount:** $518,112
- **Award type:** 1
- **Project period:** 2022-09-19 → 2024-08-31

## Primary source

NIH RePORTER: https://reporter.nih.gov/project-details/10483473

## Citation

> US National Institutes of Health, RePORTER application 10483473, Electrochemically-Controlled Rapid Chromatographic Separation of Nuisance Compounds from Natural Product Extracts (1R44AT012008-01). Retrieved via AI Analytics 2026-06-16 from https://api.ai-analytics.org/grant/nih/10483473. Licensed CC0.

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