From dietary supplements to health food products, manufacturers of nutraceutical products need to be able to verify the compositional quality of materials and identify any adulteration early on in the manufacturing process to ensure product consistency.
During the last decade, the global nutraceutical market has undergone a period of rapid growth and is now a multibillion-dollar industry. The introduction of regulations for the analysis of nutraceuticals puts manufacturers under increasing pressure to implement methods for detection that will help them to ensure compliance and protect consumer safety. Handheld Raman analysers provide a quick, accurate and reliable solution for the analysis of herbal materials and natural foods used in the manufacturing of nutraceutical products.
Regulatory compliance
As a result of the rapid growth of the nutraceuticals industry, the US Food and Drug Administration (FDA) has implemented guidelines for current Good Manufacturing Practices (cGMPs) for the manufacturing, packaging, labelling or holding operations for dietary supplements as described by the 21 CFR Part 111 standards. Manufacturers are required to follow the outlined procedures and use at least one appropriate test method to verify the material or excipient as well as confirm the identity of the final product to ensure quality control.
Furthermore, new guidelines are being developed by the United States Pharmacopeia (USP) to address issues concerning the manufacture of dietary supplements. The USP is developing these new standards in response to cases of dietary supplements being tainted with drugs. In one case, an amphetamine-like substance, BMPEA, was found in dietary supplements. Following an agreement that this product posed a risk to public health, FDA recalled the product.
The USP has subsequently developed the proposed General Chapter (2251), Adulteration of Dietary Supplements with Drugs and Drug Analogs, with the input of regulators, industry and healthcare practitioners. To reassure customers that their products meet strict standards, manufacturers must be able to accurately identify the raw materials used in herbal and natural supplements.
The nutraceutical analysis challenge
Nutraceuticals are made up of several active ingredients; incorrect formulation, contamination, mislabelled containers and counterfeit materials can result in products being 'out of specification,' which can have severe consequences for a company’s reputation. Traditionally, laboratory based test methods such as HLPC and GC have been used for the identification of these raw materials. However, these techniques involve large, expensive systems and require highly skilled operators, making it a costly process. In addition, this time consuming methodology and the complex data produced do not produce quick pass/fail results.
Internal laboratory analysis of raw materials can often take between 3 and 5 days, while results from external laboratories can take even longer, which can cause delays in the manufacturing process. Furthermore, materials must be held in a quarantine area before receiving clearance, which takes up valuable space and can cause additional delays during production.
The increasingly wide variety of materials that are used for development of nutraceuticals can prove difficult to examine using existing handheld Raman devices. Materials such as turmeric and vanadyl sulfate powder are susceptible to fluorescence when being analysed by handheld Raman units with a 532 or 785nm excitation laser.
Fluorescence interference prevents the successful identification and analysis of these materials, which prevents rapid, reliable results being provided at the point of need to ensure the authenticity of the material. All of these factors demonstrate the growing challenges with raw material analysis for the development of nutraceuticals and why there is the demand for a quick, accurate solution for raw material identification.
Benefits of implementing handheld raman
Raman spectroscopy is a recognised technique in the US and European Pharmacopoeias, and handheld Raman devices are proven to be as analytically effective as conventional lab-based methods for material identification. As a result, nutraceutical manufacturers are increasingly adopting Raman spectroscopy as a rapid and reliable identification method of unknown compounds.
Handheld Raman provides a practical and valuable solution for dietary supplement manufacturers to answer the basic question of whether materials are genuine or not, all whilst delivering improved quality control and increased production efficiency. By enabling analysis at the point of need, materials can be accepted or rejected upon receipt at the loading dock or warehouse.
This streamlines the raw material identification (RMID) workflow to allow materials to be passed through for production faster. Handheld Raman can also be used for in-process control testing during post-packaging operations, final release testing and receipt ID testing of finished goods.
Ease of use is a key factor for techniques for fast RMID and the ergonomic and rugged design of the new generation of handheld Raman has been optimised for effortlessly implementation into RMID workflows. To meet the needs of non-technical users, the new generation of handheld Raman devices has a large, easily readable angled display and single-button operation to deliver results at the point of need. Users of handheld Raman can perform ‘point and shoot’ materials analysis through some types of containers while simultaneously monitoring the measurement progress on the screen.
One of the most common frustrations for users of handheld Raman analysers with a traditional 532 or 785nm excitation wavelength is fluorescence interference when analysing materials. The introduction of handheld Raman analysers using a 1064nm excitation laser such as Progeny from Rigaku Analytical Devices enables users to overcome the issues of sample interference while maximizing efficiency. Furthermore, the 1064nm lasers also enable materials to be measured through containers such as plastic bags, thin plastic, clear glass and amber glass bottles, which helps to prevent sample contamination.
Case study
As mentioned earlier, turmeric and vanadyl sulfate can be susceptible to fluorescence interference when analysed by handheld Raman utilizing a lower excitation wavelength. To overcome this issue, in one study these two materials were measured by a handheld Raman analyser using a 1064nm wavelength excitation laser. Both materials were introduced into 2mm glass vials and were analysed with the 1064nm handheld Raman device. Using this device, it was easy to identify the materials, whereas, with a 785nm excitation laser, both materials were completely obscured by fluorescence (Figures 1 and 2).
Figure 2: Vanadyl sulfate data obtained with a handheld Raman analyser using a 1064nm wavelength excitation laser
The results of this study demonstrate the analytical advantages of using a handheld Raman 1064nm laser excitation providing fluorescence free, reliable data compared with analysers using lower excitation wavelength analysers such as 785nm.
Conclusion
Nutraceutical and dietary supplement manufacturers no longer have to rely on time-consuming, laboratory test methods to identify raw materials. By implementing handheld Raman analysers using a 1064 nm excitation laser, manufacturers can streamline their RMID workflow and be confident that they are meeting the strict regulatory requirements for material identification, whilst ultimately focusing on providing safe and reliable products to consumers.
