Tag Archives: analytical

Ask the Expert: Q&A with Steve Stadlmann on Cannabis lab Accreditation

By Aaron G. Biros
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Steve Stadlmann has an extensive background as an analytical chemist working in laboratories since the early 90’s. He is now a sales specialist at PerkinElmer, an analytical instrument manufacturer that provides instruments for cannabis testing labs, in addition to a host of other industries. With over two decades of experience working in environmental testing labs, food and beverage labs and agricultural testing labs, Stadlmann is extremely familiar with the instruments used in cannabis labs.

Steve Stadlmann, sales specialist at Perkin Elmer

In 2014, he started working in the cannabis space with TriQ, Inc., a technology solutions provider for cannabis growers, where he worked in product development on a line of nutrients. In April of 2016, he started working at Juniper Analytics, a cannabis-testing laboratory in Bend, Oregon. As laboratory director there, he created their quality manual, quality assurance plan, SOP’s and all the technical documentation for ORELAP accreditation. He developed new methodologies for cannabis testing industry for residual solvents, terpene profiles and potency analysis. He worked with PerkinElmer on pesticide methodology for the QSight™ Triple Quadrupole LC/MS/MS system and implemented operational procedures and methods for LC-UV, GCMS and LC-MS/MS, including sample prep for cannabis products.

He left Juniper Analytics about two months ago to work with PerkinElmer as a sales specialist. With extensive experience in helping get Juniper’s lab accredited, he is a wealth of knowledge on all things cannabis laboratory accreditation. PerkinElmer will be hosting a free webinar on September 12th that takes a deep dive into all things cannabis lab accreditation. Ahead of the upcoming webinar, Getting Accreditation in the Cannabis Industry, we sit down with Stadlmann to hear his observations on what instruments he recommends for accreditation, and processes and procedures to support that. Take a look at our conversation below to get a glimpse into what this webinar will discuss.

CannabisIndustryJournal: How can cannabis labs prepare for accreditation with selecting instrumentation?

Steve: Finding the appropriate instrumentation for the regulations is crucial. Ensuring the instrumentation not only has the capabilities of analyzing all the required compounds, but also able to achieve appropriate detection limit requirements. In addition, having an instrument manufacturer as a partner, that is willing and able to assist in method development, implementation and continued changes to the testing requirements at the state level (and potentially national level) is key.

Another consideration is robustness of the equipment. The instrumentation must be capable of high throughput for fast turnaround times of results. Unlike the environmental industry, the cannabis industry has consumer products with expiration dates. Clients demand quick turnaround of results to get product to market as quickly as possible and avoid sitting on inventory for any length of time.

To add to the robustness need, sample matrices in the cannabis industry can be quite challenging in relation to analytical instrumentation. Equipment that is able to handle these matrices with minimal downtime for routine service is becoming a requirement to maintain throughput needs of the industry.

CIJ: What are the most crucial procedures and practices for achieving ISO 17025 accreditation?

Steve: Development and documentation of processes and procedures following Good Laboratory Practices and procedures is essential to a successful accreditation process. Great attention must be paid to the quality objectives of the laboratory as well as associated documentation, including tracking of any errors, deviations, updates, complaints, etc.

Data integrity is a key component to any accrediting body and includes implementation and/or development of appropriate methods with support data proving acceptable results. In addition, documentation of all procedures and processes along with tracking of all steps in the process during routine laboratory work should be a priority. The ability to show a complete, documented trail of all procedures done to any sample is important in ensuring the results can be reproduced and ensuring no deviations occurred, in turn potentially causing questionable results.

Last but not least: training. Laboratory staff should be well versed in any procedures they are involved in to ensure high data quality and integrity. If any laboratory staff does not receive appropriate training in any operating procedures, the data quality becomes suspect.

CIJ: What are some of the biggest obstacles or pitfalls cannabis labs face when trying to get accredited?

Steve: Not fully preparing to meet any agency and testing regulations and requirements will cause delays in the accreditation process and potentially more work for the laboratory. From documentation to daily operations, if any aspect becomes a major finding for an auditor, additional data is usually required to prove the error has been fixed satisfactorily.

Taking the time early on to ensure all documentation, processes and procedures are adhering to any regulatory agency requirements is important for a smooth accreditation process. It is easy to overlook small details when building out the operating procedures that might be essential in the process. Again, going back to data quality, the laboratory must ensure all steps are outlined and documented to ensure high quality (reproducible) data and integrity.

A new employee should be able to come in and read a quality manual and standard operating procedure and produce equivalent data to any laboratory analyst doing the same job. With difficult or challenging operating procedures it becomes even more important that training and documentation are adhered to.

PerkinElmer’s free webinar will dive into these points and others in more detail. To learn more and sign up, click here.

The Practical Chemist

Potency Analysis of Cannabis and Derivative Products: Part 2

By Rebecca Stevens
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As mentioned in Part 1, the physiological effects of cannabis are mediated by a group of structurally related organic compounds known as cannabinoids. The cannabinoids are biosynthetically produced by a growing cannabis plant and Figure 1 details the biosynthetic pathways leading to some of the most important cannabinoids in plant material.

Potency figure 1
Figure 1: The biosynthetic pathway of phytocannabinoid production in cannabis has been deeply studied through isotopic labeling experiments

The analytical measurement of cannabinoids is important to ensure the safety and quality of cannabis as well as its extracts and edible formulations. Total cannabinoid levels can vary significantly between different cultivars and batches, from about 5% up to 20% or more by dry weight. Information on cannabinoid profiles can be used to tailor cultivars for specific effects and allows end users to select an appropriate dose.

Routine Analysis vs. Cannabinomics 

Several structurally analogous groups of cannabinoids exist. In total, structures have been assigned for more than 70 unique phytocannabinoids as of 2005 and the burgeoning field of cannabinomics seeks to comprehensively measure these compounds.¹

Considering practical potency analysis, the vast majority of cannabinoid content is accounted for by 10-12 compounds. These include Δ9-tetrahydrocannabinol (THC), cannabidiol (CBD), cannabigerol (CBG), Δ9-tetrahydrocannabivarian (THCV), cannabidivarin (CBDV) and their respective carboxylic acid forms. The cannabinoids occur primarily as carboxylic acids in plant material. Decarboxylation occurs when heat is applied through smoking, vaporization or cooking thereby producing neutral cannabinoids which are more physiologically active.

Potency Analysis by HPLC and GC

Currently, HPLC and GC are the two most commonly used techniques for potency analysis. In the case of GC, the heat used to vaporize the injected sample causes decarboxylation of the native cannabinoid acids. Derivatization of the acids may help reduce decarboxylation but overall this adds another layer of complexity to the analysis² ³. HPLC is the method of choice for direct analysis of cannabinoid profiles and this technique will be discussed further.

A sample preparation method consisting of grinding/homogenization and alcohol extraction is commonly used for cannabis flower and extracts. It has been shown to provide good recovery and precision² ³. An aliquot of the resulting extract can then be diluted with an HPLC compatible solvent such as 25% water / 75% acetonitrile with 0.1% formic acid. The cannabinoids are not particularly water soluble and can precipitate if the aqueous percentage is too high.

To avoid peak distortion and shifting retention times the diluent and initial mobile phase composition should be reasonably well matched. Another approach is to make a smaller injection (1-2 µL) of a more dissimilar solvent. The addition of formic acid or ammonium formate buffer acidifies the mobile phase and keeps the cannabinoid acids protonated.

The protonated acids are neutral and thus well retained on a C18 type column, even at higher (~50% or greater) concentrations of organic solvent² ³.

Detection is most often done using UV absorbance. Two main types of UV detectors are available for HPLC, single wavelength and diode array. A diode array detector (DAD) measures absorbance across a range of wavelengths producing a spectrum at each point in a chromatogram while single wavelength detectors only monitor absorbance at a single user selected wavelength. The DAD is more expensive, but very useful for detecting coelutions and interferences.

References

  1. Chemical Constituents of Marijuana: The Complex Mixture of Natural Cannabinoids. Life Sciences, 78, (2005), pp. 539
  2. Development and Validation of a Reliable and Robust Method for the Analysis of Cannabinoids and Terpenes in Cannabis. Journal of AOAC International, 98, (2015), pp. 1503
  3. Innovative Development and Validation of an HPLC/DAD Method for the Qualitative and Quantitative Determination of Major Cannabinoids in Cannabis Plant Material. Journal of Chromatography B, 877, (2009), pp. 4115

Rebecca is an Applications Scientist at Restek Corporation and is eager to field any questions or comments on cannabis analysis, she can be reached by e-mail, rebecca.stevens@restek.com or by phone at 814-353-1300 (ext. 2154)