By Jesse Miller, PhD, Director of Research & Development, Hemp Services, NSF International04.03.20
An accurate, reliable and reproducible testing pathway for hemp materials is imperative for farmers, processors, manufacturers and consumers. However, robust testing and safety assessments for this important crop are still in development, and manufacturers in need of testing may feel at sea when so much remains undefined. Rather than obsessing over the unresolved, manufacturers should focus on what can be measured: indicators that a testing organization will provide quality results that aid in producing a safer product for the market. Here are some key indicators that a testing facility is up to the unique challenges of the hemp marketplace.
ISO/IEC 17025 Accreditation
Because CBD products are novel and testing standards are still in development, manufacturers thirst for something—anything—to instill confidence in a testing facility. ISO/IEC accreditation helps assuage the anxiety that comes with bringing these products to market. Accreditation to ISO/IEC 17025 ensures a lab is technically competent to perform testing and calibration. It illustrates a lab’s commitment to upholding standards and quality systems and producing consistent and scientifically valid results. It is a baseline requirement for labs that operate at a standard designed to protect consumer safety and the integrity of a product’s brand.
Validated Methods
AOAC International’s Cannabis Analytical Science Program has been developing methods for a variety of different matrices; a biomass matrix is complete and one for residual solvents is underway. The goal is to develop methods that are vetted by expert scientists and that can be used industry wide. Some of the challenge comes from the sheer volume of methods required. A validation method is individualized by product, whether tablet, oil, gel capsule, gummy or any of the other constructs flooding the CBD market.
Since many of these validated methods are still under construction, confirm with a testing lab that it is following AOAC validated methods and will continuously update its testing as validated methods are approved and released. Until a complete set of validated matrices is readily available, manufacturers should confirm a testing organization’s use of current-state validated methods and how they are applied.
High-performing labs should also be able to do a method verification for specific matrices in order to provide as much accuracy as possible. Manufacturers may see irregular or inconsistent results because the validated methods for testing products simply don’t exist yet and labs may be using best-guess methods that don’t account for variables such as biomass extraction. For example, if validated methods exist for products using coconut oil, and a manufacturer’s new product contains palm oil, a lab should have the expertise to be able to do a comparative validation to ensure that the ingredient works within the reigning standard, by using a like-matrix.
Quality Control
Testing organizations should be running positive and negative controls and standards with tests so that every run provides additional information against which to compare current and future results. Every test report should provide the standards of positive/negative controls to provide essential reference data, avoiding a litany of numbers within a profile with no foundation for whether they are changing over time. Data presented in a vacuum without quality control reference is significantly less useful data.
Further, hemp is a bioaggregator and a bioaccumulator, drawing pesticides and metals from the soil and concentrating them. In addition to THC levels, testing results should include data on these and other potential adulterants. This is an argument for lot-by-lot testing as different environments produce different results for botanicals. A product’s potential benefit is meaningless if unsafe adulterant levels are present, and the interest of public health demands they be discovered and addressed before a product reaches the marketplace.
Total THC Analysis
It sounds basic, but manufacturers must know precisely how much THC is in their product, and that amount is the sum of several factors, including THC and THC acid (THCA), which is also present. If lab results don’t show a number for THCA as well as THC, or simply report total THC without breaking down the contributing factors, consider that a warning sign. A test method should provide these numbers individually and in total, and in the spirit of elementary school mathematics, labs should “show their work.” Liquid chromatography testing produces counts for both THC and THCA, offering a clear, validated process for how a lab arrives at total THC. If a lab has validated its method properly, this data is both obtainable and reportable.
Limited Detections & Limited Quantifications
Be wary of the word “nondetect,” often listed as “ND” on a test report. A test report may indicate nondetect for a chemical, but that may be because the method did not detect the target chemical. It’s misleading, as the manufacturer may think it is receiving a zero-level for a chemical when really it’s just below the limit of detection for the method. If a manufacturer is going to the expense of testing to understand the profile of a product for CBD-specific factors such as terpenes and cannabidiols (that’s why they’re in the product, after all), the test should be able to detect them, even if they are at less than 0.1%. For example, if the limit of detection is 0.05%, manufacturers may receive a report that says nondetect, because the method is not structured to detect that chemical at that level—or at all. But when that ingredient is concentrated, the manufacturer has no actual idea how much chemical it has in its product. If the initial testing comes up with a lot of nondetect numbers, concentration can unwittingly push certain cannabinoids over the lawful limit or boost the number of unsafe metals or pesticides.
An additional note about concentration: It is possible that a manufacturing process could concentrate the product in the middle of the process, and then take steps to reduce the THC so that it falls below the legal threshold. If the final product meets the less than 0.3% threshold before the process and after the process, all is well. But if the DEA or FDA decides to test a product at that high-concentration-point in the process, the risk falls on the manufacturer.
DEA License
While a DEA license is not required for the manufacturer of a dietary supplement, it is an indicator of the lab’s experience and standard reference. Consider it one of the preferred, but not required components of a testing organization’s resume. It is required for testing hemp biomass and its presence is reassuring for other products.
Claims & the FDA
The regulations are clear that dietary supplement manufacturers cannot make medical claims about their products, and yet in the first six weeks of 2020 the FDA sent multiple warning letters to manufacturers about claims of curing disease. CBD isolate has been used as a drug, but at the same time there is subtle differentiation between broad-spectrum and full-spectrum hemp extract vs. CBD isolate. Manufacturers should look for testing labs that keep a keen eye on FDA warning letters and how that may affect product marketability, especially if a product is differentiated in the market by the measurement of certain cannabinoids. As the industry develops methods, labs should also continually develop the ability to show results that support product safety and quality.
Jesse Miller, PhD, is director of research and development for Hemp Services at NSF International, a global public health and safety organization. He holds a doctorate in microbiology, with additional expertise in molecular biology and next-generation sequencing.
ISO/IEC 17025 Accreditation
Because CBD products are novel and testing standards are still in development, manufacturers thirst for something—anything—to instill confidence in a testing facility. ISO/IEC accreditation helps assuage the anxiety that comes with bringing these products to market. Accreditation to ISO/IEC 17025 ensures a lab is technically competent to perform testing and calibration. It illustrates a lab’s commitment to upholding standards and quality systems and producing consistent and scientifically valid results. It is a baseline requirement for labs that operate at a standard designed to protect consumer safety and the integrity of a product’s brand.
Validated Methods
AOAC International’s Cannabis Analytical Science Program has been developing methods for a variety of different matrices; a biomass matrix is complete and one for residual solvents is underway. The goal is to develop methods that are vetted by expert scientists and that can be used industry wide. Some of the challenge comes from the sheer volume of methods required. A validation method is individualized by product, whether tablet, oil, gel capsule, gummy or any of the other constructs flooding the CBD market.
Since many of these validated methods are still under construction, confirm with a testing lab that it is following AOAC validated methods and will continuously update its testing as validated methods are approved and released. Until a complete set of validated matrices is readily available, manufacturers should confirm a testing organization’s use of current-state validated methods and how they are applied.
High-performing labs should also be able to do a method verification for specific matrices in order to provide as much accuracy as possible. Manufacturers may see irregular or inconsistent results because the validated methods for testing products simply don’t exist yet and labs may be using best-guess methods that don’t account for variables such as biomass extraction. For example, if validated methods exist for products using coconut oil, and a manufacturer’s new product contains palm oil, a lab should have the expertise to be able to do a comparative validation to ensure that the ingredient works within the reigning standard, by using a like-matrix.
Quality Control
Testing organizations should be running positive and negative controls and standards with tests so that every run provides additional information against which to compare current and future results. Every test report should provide the standards of positive/negative controls to provide essential reference data, avoiding a litany of numbers within a profile with no foundation for whether they are changing over time. Data presented in a vacuum without quality control reference is significantly less useful data.
Further, hemp is a bioaggregator and a bioaccumulator, drawing pesticides and metals from the soil and concentrating them. In addition to THC levels, testing results should include data on these and other potential adulterants. This is an argument for lot-by-lot testing as different environments produce different results for botanicals. A product’s potential benefit is meaningless if unsafe adulterant levels are present, and the interest of public health demands they be discovered and addressed before a product reaches the marketplace.
Total THC Analysis
It sounds basic, but manufacturers must know precisely how much THC is in their product, and that amount is the sum of several factors, including THC and THC acid (THCA), which is also present. If lab results don’t show a number for THCA as well as THC, or simply report total THC without breaking down the contributing factors, consider that a warning sign. A test method should provide these numbers individually and in total, and in the spirit of elementary school mathematics, labs should “show their work.” Liquid chromatography testing produces counts for both THC and THCA, offering a clear, validated process for how a lab arrives at total THC. If a lab has validated its method properly, this data is both obtainable and reportable.
Limited Detections & Limited Quantifications
Be wary of the word “nondetect,” often listed as “ND” on a test report. A test report may indicate nondetect for a chemical, but that may be because the method did not detect the target chemical. It’s misleading, as the manufacturer may think it is receiving a zero-level for a chemical when really it’s just below the limit of detection for the method. If a manufacturer is going to the expense of testing to understand the profile of a product for CBD-specific factors such as terpenes and cannabidiols (that’s why they’re in the product, after all), the test should be able to detect them, even if they are at less than 0.1%. For example, if the limit of detection is 0.05%, manufacturers may receive a report that says nondetect, because the method is not structured to detect that chemical at that level—or at all. But when that ingredient is concentrated, the manufacturer has no actual idea how much chemical it has in its product. If the initial testing comes up with a lot of nondetect numbers, concentration can unwittingly push certain cannabinoids over the lawful limit or boost the number of unsafe metals or pesticides.
An additional note about concentration: It is possible that a manufacturing process could concentrate the product in the middle of the process, and then take steps to reduce the THC so that it falls below the legal threshold. If the final product meets the less than 0.3% threshold before the process and after the process, all is well. But if the DEA or FDA decides to test a product at that high-concentration-point in the process, the risk falls on the manufacturer.
DEA License
While a DEA license is not required for the manufacturer of a dietary supplement, it is an indicator of the lab’s experience and standard reference. Consider it one of the preferred, but not required components of a testing organization’s resume. It is required for testing hemp biomass and its presence is reassuring for other products.
Claims & the FDA
The regulations are clear that dietary supplement manufacturers cannot make medical claims about their products, and yet in the first six weeks of 2020 the FDA sent multiple warning letters to manufacturers about claims of curing disease. CBD isolate has been used as a drug, but at the same time there is subtle differentiation between broad-spectrum and full-spectrum hemp extract vs. CBD isolate. Manufacturers should look for testing labs that keep a keen eye on FDA warning letters and how that may affect product marketability, especially if a product is differentiated in the market by the measurement of certain cannabinoids. As the industry develops methods, labs should also continually develop the ability to show results that support product safety and quality.
Jesse Miller, PhD, is director of research and development for Hemp Services at NSF International, a global public health and safety organization. He holds a doctorate in microbiology, with additional expertise in molecular biology and next-generation sequencing.
