The dietary supplement industry has come under intense scrutiny from regulators and lawmakers of late—perhaps more than ever before. The investigation into herbal supplements spearheaded by New York Attorney General Eric Schneiderman last year, for example, brought questions about quality and testing protocols into the forefront, sparking debates about the utility and proper application of new, emerging technologies like DNA barcode analysis.

As a key component of a product manufacturer’s quality assurance program, proper testing is a front-line defense against economically motivated adulteration, which responsible industry players have been battling for many years. Analytical testing for identity, purity, strength and composition remains paramount to ensuring that quality products reach consumers.

Evolution of Quality
Over time, companies have realized the importance and value of testing, and product quality has improved as a direct result, according to Élan Sudberg, CEO, Alkemist Labs, Costa Mesa, CA.

Alongside the fact that testing protocols are required under federal Good Manufacturing Practices (GMPs), a strong strategy for ensuring high quality standards is simply good for the bottom line. Validation that products contain only high quality ingredients helps build trust among consumers and business partners, and ultimately trust and loyalty breed return sales, Mr. Sudberg noted.

“It protects your assets,” he said of testing. “Everything hinges on the product you make. If you’re not doing an adequate job to make sure it’s the highest quality then you’re going to have problems.”

Mr. Sudberg said his lab has seen consistent sales increases year after year, with more companies looking to conduct testing through a third-party analytical lab. In addition, the overall failure rate continues to get better, he noted, with an improvement in overall compliance.

“The majority of the samples we fail are dilution issues, meaning (for example) someone got poor quality ginkgo; it wasn’t that we found ginkgo with rat poison or something.”

What’s behind better compliance rates? It could be that companies are nervous about enforcement from federal authorities, or they’ve come to understand the true value of testing, or a combination of factors, said Mr. Sudberg. “But the fact is that compliance is on the increase for sure, and there’s no reason to believe it won’t continue that way.”

However, he also noted concern about the growing practice of skip lot testing. “The way I look at it is when I give my daughter a bite of food from my plate I make sure it’s not hot; I don’t trust the second piece is not hot and just give it to her. Skip lot testing is growing and unacceptable because it gives rise to potential failure, which—now knowing there’s more scrutiny of the industry—is more unacceptable than ever before.”

DNA Analysis
While implementation of a valid testing protocol is becoming the standard in the dietary supplement market, as opposed to a point of differentiation, DNA testing has become somewhat of a selling point, or a marketable feature, Mr. Sudberg said. That’s a positive thing, he added, as it helps communicate to consumers that products are undergoing quality checks.

After the NY AG controversy, which relied on a faulty application of the novel test method, there was an immediate spike in demand across the spectrum. “The needle went all the way to the right side toward just blindly doing DNA testing on anything and everything,” said Mr. Sudberg. “Now it’s back in the middle where it’s being discussed as its best place—where it best fits—and not as the only testing that we need to do.”

He added that DNA testing is a “very powerful tool that should be used, and used correctly.” Having made a significant investment in equipment and other resources, Alkemist will eventually be offering DNA analysis services, “because we do believe it plays a role in identity testing in this industry.” Still, other simpler, less expensive methods have been widely accepted around the world by other regulators and experts.

Perhaps the most significant obstacle to proper implementation of DNA testing for the nutraceuticals industry is finding reliable and verifiable reference materials. Ensuring the transparency and credibility of those reference standards is critical to running trustworthy and valid tests, said Mr. Sudberg.

The next step for industry will be development of a shared, public database of reference materials for companies to compare test samples to, aligning with the theme of transparency companies have been adopting, he added.

Natural Verification
When a natural product gains popularity, cheaper synthetic versions often crop up in the marketplace. In an effort to defend the purity of the curcumin supply chain, Sabinsa Corporation, East Windsor, NJ, is instituting a conclusive test to guarantee that its range of Curcumin C3 Complex products are all of natural origin.

When Sabinsa became aware that turmeric extracts adulterated with synthetic curcuminoids were infiltrating the U.S. market, the company immediately alerted its customers and the industry. Continuing the company’s proactive leadership in addressing this problem, Sabinsa initiated radio-carbon testing for all batches of Curcumin C3 Complex, safeguarding customer and consumer confidence in its product.

To distinguish synthetic curcumin from natural curcumin is not ordinarily possible through tests based on chromatography or spectral means. However, turmeric plants biosynthesize curcumin with carbon dioxide from the atmosphere as the sole carbon source. This atmospheric carbon dioxide contains extremely minuscular but accurately determinable quantities of radiocarbon (which is sometimes referred to as natural carbon).

On the other hand, synthetic curcumin is made from fossil fuel or petroleum-based materials in which radiocarbon is totally absent. Methods such as accelerator mass spectrometry can accurately assess the content of radiocarbon in a sample and can readily distinguish between a natural sample and its synthetic version. It can even determine the extent or degree of synthetic contamination in an alleged natural product when the two are mixed, which Sabinsa has identified is happening extensively in the marketplace.

Academic labs such as the Center for Applied Isotope Studies, University of Georgia, have developed reliable methods. Now several commercial labs have also adopted them and an ASTM (American Society of the International Association for Testing and Materials) method now exists that can be readily applied to curcuminoids to determine natural authenticity.

“Curcumin-based products are among the best-selling nutritive ingredients in the market today, which has given rise to highly feverish marketing and promotional activities,” said Shaheen Majeed, Sabinsa’s marketing director. “It also positions it a material ripe for economic adulteration, making it imperative that companies sourcing curcumin take steps to be sure to know exactly what they are getting, both for regulatory and brand integrity reasons.”

Curcumin is derived from the rhizome of Curcuma longa, a plant native to the Indian sub-continent and far east. The health conferring effects of curcuminoids, cited in the ancient texts of Ayurveda, are now corroborated through numerous modern scientific and clinical investigations. The main ingredient of curcumin and its relatives, demethoxycurcumin and bisdemethoxycurcumin, are also amenable to synthesis. Some companies knowingly or unwittingly market products containing synthetic curcumin, since synthetic curcumin is much cheaper to produce than plant-derived curcumin, said Mr. Majeed.

The U.S. FDA’s position on synthetic versions of natural products is that they are not the same, and require a New Dietary Ingredient (NDI) application to be legitimately sold as a nutritional ingredient.

“As industry eyes have turned to the global supply chain as the primary source of quality problems, Sabinsa continues to take action in instituting measures that deliver the safest, most efficacious ingredients possible,” Mr. Majeed said. “From warning against ‘borrowed’ science more than 20 years ago, to emphasizing the need for science to back up ingredient claims, and actively advocating IP protection, we continue to pursue the correct course for industry quality.”

Omega-3 Testing
Botanicals aren’t the only products in the nutraceuticals industry that must deal with adulteration and quality issues. Any high-priced ingredient may be at risk, according to Svein Erik Haugmo, CEO, OmegaVeritas AS, which provides laboratory services for testing authenticity of marine-based omega-3 oils. “Whenever there is money to be made by diluting the original ingredient, adulteration may occur,” he said.

For example, it’s common to brand a mixture of fish oil and cod liver oil (CLO) as pure CLO, especially in the U.K., he noted. “Some claim ‘mixture’ with small letters in the content list on the back label, while others don’t.”

As a main source of fish oil from anchovy, Peru has seen lower yields in recent years, leading to limits on fishing. “The supply from alternative sources gives rise to two main challenges: 1) is the alternative source from a sustainable fishery, and 2) is the alternative source based on the same fish species, or do brands need to re-declare their label claims?”

“To address these challenges within the marine supplement industry, we have developed a database of known reference samples, enabling us to match supplements from the shelf with our database, and tell which marine species the supplement is made of, and which part of the world the species is caught/harvested,” said Mr. Haugmo.

For example, OmegaVeritas now offers independent, third-party authenticity verification for Antarctic krill oil products—being able to verify both ingredients and end consumer products.

“For the first time, there is a laboratory test available to test the origin and authenticity of Antarctic krill oil based products,” said Mr. Haugmo. “Krill oil samples are technically challenging to analyze, but we have now established a validated system which can provide highly accurate results.”

During a year-long development project funded by Innovation Norway, OmegaVeritas developed, optimized and validated sampling procedures and logistics, analysis protocols, software algorithms as well as created a reference database. The aim was to build a system that is efficient and valid, while also ensuring integrity and transparency.

“Everything is now in place,” said Mr. Haugmo. “As a last project step and final validation, we have been collecting and analyzing commercially available krill oil products. Initial results confirm that our analysis is efficient and accurate. Also, the results are indicating that not every krill product contains what is stated on the label.”

The successful build-up of the reference database was important in contributing to accuracy. Two vertically integrated Antarctic krill oil suppliers, Aker BioMarine AS and RIMFROST AS, were the industry partners in this project and crucial in providing authentic reference samples. Having their own vessels and ability to fully trace batches to the precise krill harvesting times and locations was important for ensuring a large enough spectrum of authentic samples—from different times and geographical origins.

The authenticity-testing tool for Antarctic krill oil is now commercially available.

“We are at risk of losing money every day due to adulterated products,” said RIMFROST CEO John Cameron. “With strong support from the industry, OmegaVeritas has now developed a tool for purchasers that will assist in isolating products that are 100% authentic krill oil.”

Matts Johansen, CEO of Aker BioMarine AS, noted, “As often happens with successful, premium ingredients, the krill oil category risks being attacked by suppliers with adulterated, low-cost products. The result of this project is a third-party verification service, which might prevent this adulteration from happening.”

OmegaVeritas offers subscription programs with random analysis and mandatory next-level-in-value-chain checkpoints, batch certifications, product verifications (with possibility to use the verification logo on the label), as well as product screening and benchmarking. All services have special sampling routines solving third-party sampling challenges. Eventually there will be a wide range of offers servicing different value chain actors—including retailers and consumers.

Whether it’s omega-3s, herbal supplements, or specialty ingredients like chondroitin and other nutraceuticals, proper analytical methods will continue to weed out economically motivated adulteration while protecting companies that aim to deliver quality products.