Tag Archives: chemical

Quality Assurance In The Field: Instruments For Growers & Processors

By Aaron G. Biros
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As the cannabis marketplace evolves, so does the technology. Cultivators are scaling up their production and commercial-scale operations are focusing more on quality. That greater attention to detail is leading growers, extractors and infused product manufacturers to use analytical chemistry as a quality control tool.

Previously, using analytical instrumentation, like mass spectrometry (MS) or gas chromatography (GC), required experience in the laboratory or with chromatography, a degree in chemistry or a deep understanding of analytical chemistry. This leaves the testing component to those that are competent enough and scientifically capable to use these complex instruments, like laboratory personnel, and that is still the case. As recent as less than two years ago, we began seeing instrument manufacturers making marketing claims that their instrument requires no experience in chromatography.

Instrument manufacturers are now competing in a new market: the instrument designed for quality assurance in the field. These instruments are more compact, lighter and easier to use than their counterparts in the lab. While they are no replacement for an accredited laboratory, manufacturers promise these instruments can give growers an accurate estimate for cannabinoid percentages. Let’s take a look at a few of these instruments designed and marketed for quality assurance in the field, specifically for cannabis producers.

Ellutia GC 200 Series

Shamanics, a cannabis extractor in Amsterdam, uses Ellutia’s 200 series for QA testing

Ellutia is an instrument manufacturer from the UK. They design and produce a range of gas chromatographs, GC accessories, software and consumables, most of which are designed for use in a laboratory. Andrew James, marketing director at Ellutia, says their instrument targeting this segment was originally designed for educational purposes. “The GC is compact in size and lightweight in stature with a full range of detectors,” says James. “This means not only is it portable and easy to access but also easy to use, which is why it was initially intended for the education market.”

Andrew James, marketing director at Ellutia

That original design for use in teaching, James says, is why cannabis producers might find it so user-friendly. “It offers equivalent performance to other GC’s meaning we can easily replace other GC’s performing the same analysis, but our customers can benefit from the lower space requirement, reduced energy bills, service costs and initial capital outlay,” says James. “This ensures the lowest possible cost of ownership, decreasing the cost per analysis and increasing profits on every sample analyzed.”

Shamanics, a cannabis oil extraction company based in Amsterdam, uses Ellutia’s 200 series for quality assurance in their products. According to Bart Roelfsema, co-founder of Shamanics, they have experienced a range of improvements in monitoring quality since they started using the 200 series. “It is very liberating to actually see what you are doing,” says Roelfsema. “If you are a grower, a manufacturer or a seller, it is always reassuring to see what you have and prove or improve on your quality.” Although testing isn’t commonplace in the Netherlands quite yet, the consumer demand is rising for tested products. “We also conduct terpene analysis and cannabinoid acid analysis,” says Roelfsema. “This is a very important aspect of the GC as now it is possible to methylate the sample and test for acids; and the 200 Series is very accurate, which is a huge benefit.” Roelfsema says being able to judge quality product and then relay that information to retail is helping them grow their business and stay ahead of the curve.

908 Devices G908 GC-HPMS

908 Devices, headquartered in Boston, is making a big splash in this new market with their modular G908 GC-HPMS. The company says they are “democratizing chemical analysis by way of mass spectrometry,” with their G908 device. That is a bold claim, but rather appropriate, given that MS used to be reserved strictly for the lab environment. According to Graham Shelver, Ph.D., commercial leader for Applied Markets at 908 Devices Inc., their company is making GC-HPMS readily available to users wanting to test cannabis products, who do not need to be trained analytical chemists.

The G908 device.

Shelver says they have made the hardware modular, letting the user service the device themselves. This, accompanied by simplified software, means you don’t need a Ph.D. to use it. “The “analyzer in a box” design philosophy behind the G908 GC-HPMS and the accompanying JetStream software has been to make using the entire system as straightforward as possible so that routine tasks such as mass axis calibration are reduced to simple single actions and sample injection to results reporting becomes a single button software operation,” says Shelver.

He also says while it is designed for use in the field, laboratories also use it to meet higher-than-usual demand. Both RM3 Labs in Colorado, and ProVerde in Massachusetts, use G908. “RM3’s main goal with the G908 is increased throughput and ProVerde has found it useful in adding an orthogonal and very rapid technique (GC-HPMS) to their suite of cannabis testing instruments,” says Shelver.

Orange Photonics LightLab Cannabis Analyzer

Orange Photonics’ LightLab Cannabis Analyzer

Dylan Wilks, a third generation spectroscopist, launched Orange Photonics with his team to produce analytical tools that are easy to use and can make data accessible where it has been historically absent, such as onsite testing within the cannabis space. According to Stephanie McArdle, president of Orange Photonics, the LightLab Cannabis Analyzer is based on the same principles as HPLC technology, combining liquid chromatography with spectroscopy. Unlike an HPLC however, LightLab is rugged, portable and they claim you do not need to be a chemist to use it.

“LightLab was developed to deliver accurate repeatable results for six primary cannabinoids, D9THC, THC-A, CBD, CBD-A, CBG-A and CBN,” says McArdle. “The sample prep is straightforward: Prepare a homogenous, representative sample, place a measured portion in the provided vial, introduce extraction solvent, input the sample into LightLab and eight minutes later you will have your potency information.” She says their goal is to ensure producers can get lab-grade results.

The hard plastic case is a unique feature of this instrument

McArdle also says the device is designed to test a wide range of samples, allowing growers, processors and infused product manufacturers to use it for quality assurance. “Extracts manufacturers use LightLab to limit loss- they accurately value trim purchases on the spot, they test throughout their extraction process including tests on spent material (raffinate) and of course the final product,” says McArdle. “Edibles manufacturers test the potency of their raw ingredients and check batch dosing. Cultivators use LightLab for strain selection, maturation monitoring, harvesting at peak and tinkering.”

Orange Photonics’ instrument also connects to devices via Wi-Fi and Bluetooth. McArdle says cannabis companies throughout the supply chain use it. “We aren’t trying to replace lab testing, but anyone making a cannabis product is shooting in the dark if they don’t have access to real time data about potency,” says McArdle.

Steep Hill Hawaii Launches, Receives ISO 17025 Accreditation

By Aaron G. Biros
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Spectra Analytical LLC, doing business as Steep Hill Hawaii, was the first cannabis-testing laboratory to be licensed by the State of Hawaii and opened for business on August 1st. Today the lab announced they received ISO 17025:2005 certifications in biological and chemical testing from Perry Johnson Laboratory Accreditation, Inc., according to a press release.

Dana Ciccone, chief executive officer of Steep Hill Hawaii, has been a patient advocate and leader in cannabis education in Hawaii, as well as a member of the Hawaii Medical Marijuana Dispensary Task Force, an organization formed by the University of Hawaii College of Social Sciences Public Policy Center to develop regulations for the state. “We are proud not only to be the first cannabis lab to be licensed in the State of Hawaii, but also now the first lab to achieve ISO certification as well,” says Ciccone. “Industry businesses, medical professionals, state regulators, and patients can be confident that our lab and its testing standards will operate to the highest international standards.”

According to the press release, the laboratory will offer services for testing cannabinoid profiles (potency), terpenes, pesticides, heavy metals, biological screening, and residual solvents, testing for 17 Cannabinoids and 43 terpenes. The release states they are locally owned and operated, providing testing services for not just industry businesses, but in-state card-holding patients as well.

“This is a turning point for the industry – we have moved very quickly to raise the industry standards in Hawaii to internationally recognized certification,” says Ciccone. “I am very proud our scientific team for the professionalism and hard work they put in to achieve this certification.”

Annual AOCS Meeting Spotlights Cannabinoid Analytics

By Aaron G. Biros
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The AOCS Annual Meeting is an international science and business forum on fats, oils, surfactants, lipids and related materials. The American Oil Chemist’s Society (AOCS) is holding their meeting in Orlando, Florida from April 30 to May 3, 2017. Last year’s meeting included discussions on best practices and the pros and cons of different extraction techniques, sample preparation, proficiency testing and method development, among other topic areas.

Posters on display for the duration of the Annual Meeting will discuss innovative solutions to test, preparing samples, discovering new compounds and provide novel information about the compounds found in cannabis. David Egerton, vice president of technical operations at CW Analytical (a cannabis testing laboratory in Oakland, CA), is preparing a poster titled Endogenous Solvents in Cannabis Extracts. His abstract discusses testing regulations focusing on the detection of the presence of solvents, despite the fact that endogenous solvents, like acetone and lower alcohols, can be found in all plant material. His study will demonstrate the prevalence of those compounds in both the plant material and the concentrated oil without those compounds being used in production.rsz_am17-editorialpic-cij

The conference features more than 650 oral and poster presentations within 12 interest areas. This year’s technical program includes two sessions specifically designed to address cannabinoid analytics:

Lab Proficiency Programs and Reference Samples

How do you run a lab proficiency program when you cannot send your samples across state lines? What constituents do you test for when state requirements are all different? Are all pesticides illegal to use on cannabis? What pesticides should be tested for when they are mostly illegal to use? How do you analyze proficiency results when there are no standard methods? Learn about these and other challenges facing the cannabis industry. This session encourages open and active discussion, as the cannabis experts want to hear from you and learn about your experiences.

Method Development

The need for high-quality and safe products has spurred a new interest in cannabinoid analytics, including sample preparation, pesticide, and other constituent testing. In this session, a diverse group of scientists will discuss developing analytical methods to investigate cannabis. Learn the latest in finding and identifying terpenes, cannabinoids, matrix effects, and even the best practice for dissolving a gummy bear.

Cynthia Ludwig speaking at last year's meeting
Cynthia Ludwig speaking at last year’s meeting

Cynthia Ludwig, director of technical services at AOCS, says they are making great progress in assembling analytical methods for the production of the book AOCS Collection of Cannabis Analytical Methods. “We are the leading organization supporting the development of analytical methods in the cannabis industry,” says Ludwig. “Many of the contributors in that collection will be presenting at the AOCS Annual Meeting, highlighting some of the latest advances in analyzing cannabis.” The organization hopes to foster more collaboration among those in the cannabis testing industry.

In addition to oral and poster sessions, the 2017 Annual Meeting will feature daily networking activities, more than 70 international exhibitors, two special sessions, and a Hot Topics Symposia which will address how current, critical issues impact the future of the fats and oils industry.

The Practical Chemist

Building the Foundation of Medical Cannabis Testing – Understanding the Use of Standards and Reference Materials – Part 2

By Joe Konschnik
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In the last article I referred to the analogy of the analytical reference material being a keystone of the laboratory foundation, the stone upon which all data relies. I then described the types of reference materials and their use in analytical testing in general terms. This article will describe the steps required to properly manufacture and deliver a certified reference material (CRM) along with the necessary documentation.

A CRM is an exclusive reference material that meets strict criteria defined by ISO Guide 34 and ISO/IEC 17025.  ISO is the International Organization for Standardization and IEC is the International Electrotechnical Commission. These organizations work together to set globally recognized standards. In order for a reference material to be labeled as a CRM it must 1) be made with raw or starting materials which are characterized using qualified methods and instruments, 2) be produced in an ISO-accredited lab under documented procedures, and 3) fall under the manufacturer’s scopes of accreditation. Verifying a CRM supplier has these credentials is easily done by viewing their certificates which should include their scopes of accreditation. Restek_accredit

There are many steps required to produce a CRM that meets the above three criteria.  The first step requires a review of the customer’s, or end-user’s requirements to carefully define what is to be tested, at what levels and which analytical workflow will be used.  Such information enables the producer to identify the proper compounds and solvents required to properly formulate the requested CRM.

The next step requires sourcing and acquiring the raw, or starting materials, then verifying their compatibility and stability using stability and shipping studies in accordance with ISO requirements. Next the chemical identify and purity of the raw materials must be characterized using one or more analytical techniques such as: GC-FID, HPLC, GC-ECD, GC-MS, LC-MS, refractive index and melting point. In some cases, the percent purity is changed by the producer when their testing verifies it’s different from the supplier label. All steps are of course documented.

restek_CRMThe producer’s analytical balances must be verified using NIST traceable weights and calibrated annually by an accredited third party provider to guarantee accurate measurement. CRMs must be prepared using Class A volumetric glassware, and all ampules and vials used in preparation and final packaging must be chemically treated to prevent compound degradation during storage. Next, CRMs are packaged in an appropriate container, labeled then properly stored to maintain the quality and stability until it’s ready to be shipped. All labels must include critical storage, safety and shelf life information to meet federal requirements. The label information must be properly linked to documentation commonly referred to as a certificate of analysis (COA) which describes all of the above steps and verifies the traceability and uncertainty of all measurements for each compound contained in the CRM. Restek_CRM2

My company, RESTEK, offers a variety of documentation choices to accompany each CRM. Depending on the intended use and data quality objectives specified by the end-user, which were defined way back at the first step, three options are typically offered: They include gravimetric only, qualitative which includes gravimetric, and fully quantitative which includes all three levels of documentation. The graphic to the right summarizes the three options and what they include.

It’s important to understand which level you’re purchasing especially when ordering a custom CRM from a supplier. Most stock CRMs include all three levels of documentation, but it’s important to be sure.

Understanding what must be done to produce and deliver a CRM sets it apart from other reference material types, however it’s important to understand there are some instances where CRMs are either not available, nor required and in those situations other types of reference materials are perfectly acceptable.

If you have any questions or would like more details about reference materials please contact me, Joe Konschnik at (800) 356-1688 ext. 2002 by phone, or email me at joe.konschnik@restek.com.

Steep Hill Labs Expands to Pennsylvania, Washington, D.C.

By Aaron G. Biros
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Last week, Steep Hill Labs, Inc. announced plans to expand on the East Coast, including licensing for laboratories in Washington, D.C. and Pennsylvania. The cannabis testing company now is operating or developing in seven states, the District of Columbia along with an official arrangement with a research university in Jamaica, according to Cathie Bennett Warner, director of public relations at Steep Hill.

The same team of physicians that oversees the Steep Hill laboratory in Maryland will operate the Pennsylvania and D.C. labs. Heading that team is chief executive officer Dr. Andrew Rosenstein, chief of the division of Gastroenterology at University of Maryland Saint Joseph Medical Center and assistant clinical professor of Gastroenterology and Hepatology at the University of Maryland Medical Center. Dr. Rosenstein has been recognized by Baltimore Magazine as a top doctor in the Baltimore area, according to a press release.

Dr. Andrew Rosenstein, CEO of Steep Hill Maryland, PA and D.C.
Dr. Andrew Rosenstein, CEO of Steep Hill Maryland, PA and D.C.

According to Dr. Rosenstein, they want to provide accurate clinical results for trials with patients using cannabis. “All clinical trials will require a competent, credible and reliable lab partner and that is what we are bringing to the field- and that is why we are working with Steep Hill,” says Dr. Rosenstein. With team members having backgrounds in pathology, molecular diagnostics, clinical chemistry, microbiology and genetics, it should come as no surprise that they plan to participate in clinical research.

Dr. Rosenstein’s vested interest in cannabis safety stems from prior experience with his patients using cannabis. “Over the past five years, we have seen an increased number of patients using cannabis, particularly for managing the side effects of Crohn’s disease and cancer treatment,” says Dr. Rosenstein. “They would bring it up to us and at the time I didn’t know much about it, but anecdotally it’s really clear that a lot of patients have great responses to it.” Not knowing much about the preparation or safety of cannabis at the time led Dr. Rosenstein to advise patients to be very careful if they are immunocompromised.

Examination of cannabis prior to testing- credit Steep Hill Labs, Inc.
Examination of cannabis prior to testing- credit: Steep Hill Labs, Inc.

“When a patient is immunocompromised, a bacterial or fungal infection can be lethal, so because we had patients using cannabis, we wanted to make sure it was safe,” says Dr. Rosenstein. So when Maryland legalized medical cannabis, Dr. Rosenstein and his team saw the need to protect patient safety and Steep Hill was a perfect fit. “We really didn’t want to reinvent the wheel so we looked for someone to partner with,” says Dr. Rosenstein. “Steep Hill has the best technology and the best credibility and we didn’t want to compromise on quality and safety issues. They felt the same way so we partnered with them and culturally it has been a great fit.”

Steep Hill Express in Berkeley, CA- MD,PA and D.C. will have a similar offering of instant potency analysis
Steep Hill Express in Berkeley, CA- MD,PA and D.C. will have a similar offering of instant potency analysis

The new laboratories plan to offer a similar range of services that are offered at other Steep Hill labs, such as rapid potency testing for THC-A, ∆-9-THC, CBD, CBD-A and moisture. But Dr. Rosenstein sees clinical opportunities in the East Coast medical hubs. “We want to provide the testing component for studies, providing clinical reproducibility and consistency, and those are the things as a top-notch lab that we are interested in doing.”

A petri dish of mold growth from tested cannabis- Photo credit: Steep Hill-
A petri dish of mold growth from tested cannabis- Photo credit: Steep Hill Labs, Inc.

With a physician-led group that has experience in molecular diagnostics, partnering with Steep Hill is about being medically focused, according to Dr. Rosenstein. “First and foremost, this is about patient safety.” Because of that, he emphasizes the need for required microbiological contaminant testing, particularly because of his experience with patients. “If you’re a cancer patient and you get a toxic dose of salmonella or E. coli, that can kill you, so testing for microbiologic  contamination is of the highest priority.”

According to Warner, bridging the medical cannabis science gap with Steep Hill’s professionalism and experienced doctors practicing medicine is a big deal. “We are working very closely with their medical team to make sure these standards are medically superior,” says Warner. “To have these doctors with such a high level of knowledge in medicine working with us in cannabis analytics is a breakthrough.”

Automated Solutions for Cannabis Laboratories: Part I

By Danielle Mackowsky
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rsz_96_well_plate-1-1
Using well plates for dSPE sorbents can help expedite sample clean up.

Sample volume remains to be the primary influence on whether an automated solution is a logical investment for a cannabis testing facility. Due to both the complexity of the material being tested and the extraction approach at hand, it may be difficult to find an automated platform that can fully accommodate your laboratory’s needs. Hamilton Robotics in collaboration with United Chemical Technologies (UCT) has developed a solution that allows for automation of specific sample clean up steps commonly utilized in cannabis pesticide testing schemes. The MPE2 Positive Pressure Extraction/Evaporation Module is a standalone manifold that can also be incorporated into a number of automated liquid handling decks. Used in tandem with dispersive solid phase extraction (dSPE) salts/sorbents packed into a 96 well plate, this combination provides laboratories with high throughput extraction convenience with comparable results to traditional dSPE for the analysis of over forty pesticides.

As states continue to expand testing requirements for pesticides, it is vital that your laboratory is equipped with a method that allows versatility for the addition of new compounds without burdening your extraction team. There are a variety of dSPE salt and sorbent blends readily available that have been optimized for cannabis extractions. This allows for the use of a reliable extraction technique that can be adapted for the automation age. Hamilton is widely recognized throughout both clinical and forensic laboratory settings and the MPE2 platform is an excellent first system for laboratories beginning to automate/semi-automate their processes.

MPE2 Positive Pressure Extraction/Evaporation Module
MPE2 Positive Pressure Extraction/Evaporation Module

Following an initial QuEChERS extraction, additional cleanup is typically recommended for extracts that are being analyzed for pesticide content due to the low detection limits often required. dSPE provides the necessary sample clean up to obtain those thresholds, but often burdens a laboratory staff with additional time consuming preparation steps. Traditionally, dSPE salts are packed into 2 mL centrifugation tubes that require a cumbersome supernatant pipetting step followed by additional vortex, spin and transfer steps. By packing the dSPE sorbents into a well plate format, the user is able to completely automate this above described clean up ultimately saving time and adding convenience without jeopardizing any recovery data.

For most compounds, the recovery was greater than 65% for both methods of dSPE. The mean recoveries for traditional dSPE were 98.0%, 99.2% and 97.9% at pesticide concentrations of 50 ng/mL, 100 ng/mL and 200 ng/mL, respectively. For comparison, the mean recoveries at the same concentrations for well plate dSPE were 85.0%, 88.9% and 89.1%. Therefore, there was typically about a 10-11% absolute difference in recovery between the two methods, which can be corrected for by implementing the use of internal standards. When comparing the recovery differences between the two methods, there are six compounds with noticeably larger discrepancies across all three concentrations, namely: chlorpyrifos, cyprodinil, diazinon, spinetoram, spiromesifen 278 and trifloxystrobin. If these data sets are excluded, then the average absolute differences in recovery between the two methods decrease to 8.8%, 6.4% and 5.8% for concentrations of 50 ng/mL, 100 ng/mL and 200 ng/mL, respectively.rsz_1shutterstock_226135945-1

Overall, laboratories can estimate on saving 40-60 minutes per 96 samples processed using the Hamilton MPE2 in conjunction with a UCT dSPE plate. When a liquid handling robot is also available, this time saving estimation is potentially doubled. Time spent per sample, including the training of laboratory scientists, is an important factor to consider when setting up your laboratory. Automation is in an investment that can greatly reduce a laboratory’s overall labor costs in the long run.

Tech Startup Seeking Investors for Cannabis Data Research Tool

By Aaron G. Biros
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Innovations in technology used for cannabis research have the potential to lead to major breakthroughs and discoveries for the plant’s various applications. Software and information technologies are particularly useful for sorting through the tremendous amount of data required in medical research and the cannabis industry. Tímea Polgár, founder of CannaData, worked in the pharmaceutical and biotech industries previously as a molecular biologist and computational chemist.

Tímea Polgár, founder of CannaData
Tímea Polgár, founder of CannaData

Her background in informatics, pharmaceutical research, molecular biology and chemistry brings her to the cannabis industry to study the plant in an herbal medicine context using high-tech informatics. Polgár, originally from Hungary, received her PhD from Budapest University of Technology and Engineering in pharmaceutical drug discovery. She has worked as a senior research scientist at Gedeon Richter in Budapest and as a senior molecular modeler at Servier, Inc. in Paris, France. After leaving the pharmaceutical industry, she began working at a startup called Chemaxon, a chemistry informatics company working on scientific business development. Polgár has worked for years in scientific business development, leveraging technology and knowledge to businesses, which brought her to work across multiple disciplines.

CannaData is essentially a software tool used to gather information on strain genetics, chemical components of different strains, molecular mechanisms of different strains and the medicinal effects. According to Polgár, the company plans to build a continuously growing data repository in conjunction with computational modeling and research in determining entourage effects to pinpoint how active chemical agents in cannabis interact. The tool will help scientists find areas of the plant that need more studying and areas that are inert. In addition to the database, CannaData will provide scientific analysis of data from seed banks, laboratories, clinics and other businesses collecting data in the cannabis industry.

A flowchart of the scientific concept behind herbal medicine research
A flowchart of the scientific concept behind herbal medicine research

Polgár’s organization is currently seeking investors to launch the project in hopes of connecting the cannabis industry, herbal medicine and computational chemistry for more accurate scientific research and understanding of the plant. According to Polgár, research and development of disease-fighting drugs has long had a narrow-minded approach. “Herbal medicine is very complex with numerous active chemical components. Recent technological and computational advancements have made it possible to study these chemical network interactions,” says Polgár. “The cannabis industry could provide a pioneering route for the novel concept of combining herbal medicinal research with information technology, furthering our molecular understanding of the benefits of cannabis.”

A flowchart breaking down the chemical composition of cannabis
A flowchart breaking down the chemical composition of cannabis

Polgár believes that this type of research has the ability to help support standardization and quality control in the cultivation of cannabis. “We are linking technologies to herbal medicine and cannabis where there is a huge need to manage, extract and analyze data,” says Polgár. “Today, there are computational technologies that can manage this quantity of information required to model and understand herbal molecular mechanisms and we will be the first ones to do so on a commercial level.”

A flowchart describing the technical concept of CannaData, depicting the utility of a data repository
The technical concept of CannaData, depicting the utility of a data repository

Polgár’s organization is seeking investors looking to innovate in the areas of life sciences, pharmaceutical research and software development. Through bringing broad information technological solutions from research to the cannabis industry, CannaData hopes to serve analytical laboratories with chemical informatics software services. Ultimately, this project will serve the cannabis industry by analyzing data on strain genetics and known chemical profiles of cannabis, furthering scientific research on cannabis.