The combination of Fourier transform infrared (FTIR) spectroscopy with attenuated total reflectance (ATR) was found to detect the presence of known adulterants, including erectile dysfunction drugs, steroids, weight loss drugs and Melamine.
The test requires only thirty seconds grinding in an analytical mill prior to the scan, which itself takes less than 10 minutes, according to a report by NOW Foods’ Andrea Champagne and Katrina Emmel in the peer-review journal Vibrational Spectroscopy.
“The method utilizes existing equipment and software, is easy to use, requires minimal sample preparation, does not require data interpretation, can be performed by non-technical personnel, has a short run time and is functional across a wide range of raw materials and adulterants,” wrote Champagne and Emmel.
Indeed, Michael Lelah, technical director at NOW Foods, told NutraIngredients-USA that they have not found any raw material formats or adulterant types for which the test does not work.
The issue
Deliberate adulteration of products continues to be an issue for the dietary supplements industry and can be either economically motivated adulteration (EMA) or to ‘intensify a desired pharmacological effect’, explained Champagne and Emmel.
The GMP regulations are widely accepted as a big step in the right direction: The 2007 GMP regulations place the onus on product manufacturers to ensure the quality of their raw materials is sufficient.
Adulteration does still occur, however, and notable examples include adulteration with erectile dysfunction drugs, weight-loss drugs, melamine, and steroid compounds. Such issues have led some critics to suggest that dietary products are ‘unregulated’. Lelah said the new rapid screening test “can help change this perception”.
The test
According to the paper in Vibrational Spectroscopy, the test uses ATR in combination with FTIR. ATR is a technique requires minimal-to-no sample preparation and allows the sample to be examined directly in the gas, liquid, or solid state. The NOW Foods scientists used a PerkinElmer FTIR Spectrum One spectrometer equipped with a universal ATR sampling system with a single bounce ZnSe/diamond crystal.
The test was applied to 84 raw ingredient chosen from a variety of product categories, including weight management, sports nutrition, men’s virility, and protein-based products. Mathematical comparisons using appropriate software produces a report bearing a ‘Pass/Fail’ assessment.
Moving forward
“This method is adaptable to new concerns and new raw materials, providing even greater flexibility and utility,” wrote Champagne and Emmel.
“Additional studies are being conducted to determine if a microspectroscopy method could be able to provide even lower detectable concentrations on raw material samples. Further investigation into the applications of PCA or LDA is also being conducted.”
Lelah confirmed that these studies are indeed underway, but there have been no new updates.
Industry acceptance
Commenting on the new rapid test, Michael Lelah said the company hopes the industry will consider using the approach to test for adulteration in their ingredients. “NOW Foods has been using this tool for over a year to inspect sports supplement ingredients. It has insured that no adulterated products reached the marketplace,” added Lelah.
The method has been shared with a variety of association FDA, AHPA, NPA, ABC, and NIH, said NOW Foods.
Speaking to NutraIngredients-USA.com, Cara Welch, PhD, scientific and regulatory affairs manager for the Natural Products Association (NPA) said she was "excited to see a paper like this coming out on behalf of the industry.
"The screening test is very applicable to industry, and the detection limits do cover the deliberate adulteration aspects," added Dr Welch.
Source: Vibrational Spectroscopy
Published online ahead of print, doi: 10.1016/j.vibspec.2010.11.009
“Rapid screening test for adulteration in raw materials of dietary supplements “
Authors: A.B. Champagne, K.V.Emmel