Analytical methods are spotlighted when a botanical’s new popularity raises the specter of adulteration, but more generally help assure that that the ingredient is the genuine article.

The months-long controversy over DMAA (1,3-dimethylamylamine) can be seen as a poster child for the importance of validated analytical methods. This past April, the Food and Drug Administration (FDA) issued warning letters to 10 manufacturers and distributors, telling them to stop selling DMAA-containing geranium oil supplements on grounds of “marketing products for which evidence of the safety of the product has not been submitted to the FDA.” FDA said that DMAA could increase blood pressure and therefore increase the risk of “a cardiovascular event.” 

Testing labs, both independent and inhouse, have maintained that DMAA does not occur naturally in geranium oil, and that therefore products containing the ingredient have been adulterated. James Neal-Kababick, director of Oregonbased Flora Research Laboratories, told the website Nutraingredients.com that FDA’s crackdown was the “end of a long run for DMAA” and was unsurprising in view of credible research that “has failed to indicate any detectable DMAA in geranium oil even using the power of a research grade, high-resolution gas chromatography- mass spectroscopy [GC-MS] instrument.” 

Two months later, the website reported a study, also conducted with GC-MS as well as liquid chromatography–highresolution mass spectrometry, that appeared to settle the matter. Writing in the Journal of Analytical Toxicology, a team from several research institutes— including the United States Anti-Doping Agency—affirmed that analytical methods could not detect measurable quantities of DMAA in geranium oil.

A study in Complementary Therapies in Medicine this past March concluded that more widespread use of analytical methods was among a number of steps the industry should take in view of a stillsizable number of adverse events from herbal supplements. It’s a point with which Michael Lelah, technical director for Illinois-based NOW Foods and its ingredient arm, Healthco, would agree.

“When ingredients are in short supply, either because they are popular (demand) or due to a poor crop (supply), they become targets for adulteration,” said Lelah. “At NOW Foods, we monitor this and, in many cases, have stepped up adulteration testing in response to specific issues.” 

The company analyzes all of its botanical ingredients, Lelah said. “Our raw material botanicals are all analyzed for identity, potency (when a specific marker exists) and purity (i.e. contamination and adulteration),” he explained.NOW also analyzes its finished product botanicals), again when a marker exists.

“Most standardized botanicals have a specific marker, such as ginkgoflavonglycosides in ginkgo biloba extract,” Lelah said. “But some botanicals—for example, whole botanicals, mushrooms and crops—don’t have specific markers, so they are not analyzed for potency.” 

Similarly, botanical ingredient supplier Gencor Pacific (with U.S. offices in Texas and California) analyzes all of its ingredients for all of the tests given in its certificates of analysis and does that for every batch of every ingredient, said R. V. Venkatesh, the company’s managing director. “We follow pharmaceutical GMP standards in manufacturing, quality control, quality assurance and analysis methodology.” 

It’s A Must 

Both Venkatesh and Lelah pointed out that with the advent of dietary supplement good manufacturing practices (GMPs), long sought by the industry, analyzing every batch of every ingredient for all tests mentioned in the product specifications is now a must. “We have developed and validated analytical methodologies for every ingredient that is produced and sold by our group,” said Venkatesh.

“The FDA dietary supplement GMPs have taken the analysis of botanicals from something that only the better manufacturers did to a requirement for all products,” added Lelah. “NOW Foods has been analyzing our botanicals for many years, but we have stepped up our analysis to cover all the requirements of the GMPS.” 

Other factors that have put the spotlight on analysis include adulteration and spiking with pharmaceuticals, Lelah said.NOW Foods conducts adulteration screening—for example, the company’s analytical lab can identify the presence of steroids, Viagra analogs and weightloss drugs—for a number of botanicals.

“Another challenge is the difficulty of analyzing for botanicals in a complex mixture,” he added. “The new GMPs require that finished products also be analyzed, but this is a big challenge for our analytical scientists.” 

Helping to lighten the load on scientists are programs such as the Botanical Authentication Program of the American Herbal Products Association (AHPA).Now 15 years old, the program identifies herbs and potential adulterants that are known to be in trade. The list identifies safety-related substitutions, among them Digitalis lanata leaf for plantain (Plantago lanceolata) leaf, and safety- and economic- based substitutions, such as red dye #2 (amaranth dye) for bilberry fruit extract. All of this information can be found on AHPA’s website.

At the start of this year, AHPA added analytical methods for the identification of star anise fruit (Illicium verum) to this Botanical Authentication Program. The intent is to differentiate it from the fruit of other Illicium species that are toxic, such as Japanese star anise (Illicium anisatum), long known to contain toxic principles.

“The industry is quite capable of obtaining the genuine article, and adulteration of this ingredient appears to be exclusively at the retail level when the wrong species is chosen and used as a traditional remedy,” said Steven Dentali, PhD, AHPA’s chief science officer.“Providing means to clearly identify ingredients where an issue of safety or economic adulteration may occur is something we believe will greatly assist our members and the industry.” 

AHPA’s Botanical Authentication Program offers two components: identification of known adulterants and information on analytical methods that can be used to ensure botanical identity.With star anise added to the roster, AHPA now provides methods of ingredient identification and analysis for five herbal ingredients, one toxic botanical constituent and one non-botanical supplement ingredients.Aside from star anise, they include: aristolochic acid; bilberry (Vaccinium myrtillus) fruit extract; black cohosh (Actaea racemosa syn. Cimicifuga racemosa) root/rhizome; eleuthero (Eleutherococcus senticosus) root; hoodia gordonii stem; and glycerin.

Some branded ingredient suppliers have branded analytical programs. At Verdure Sciences in Indiana, for example, the company employs its trademarked VBATS (Verdure Botanical Active Testing System) as a tool in its product development.Verdure said the program “enriches our understanding of botanical extracts by offering intimate analysis of their underlying chemistry, activity and quality.” 

In order to do so, Verdure turns to experts in various specialties within chemistry, biology and medicine at leading universities throughout North America and overseas. Similarly, the company looked to an independent panel of outside experts in support of a GRAS determination for its Longvida® Optimized Curcumin, following more than a dozen preclinical studies on the ingredient as well as scores on curcumin by a number of government and university research groups.

FOR MORE INFORMATION:

American Herbal Products Association,(301) 588-1171  
Gencor Pacific, (714) 870-8723  
Healthco/NOW Foods, (800) 477-3949  
Verdure Sciences, (317) 776-3600