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SiliCycle Products for Cannabis Analysis

The cannabis market has experienced rapid growth over the last 20 years with more and more countries legalizing its products. With its popularity has come more sophisticated production methods as well as analytical quality control.

Of key interest are two parallel segments growing in tandem: recreational and medical canabis. While there are more than a hundred cannabinoids identified in cannabis, the current molecules of interests in these are segments are THC (tetrahydrocannabinol), CBD (cannabidiol), CBG (cannabigerol) and CBN (cannabiol).

Cannabis analysis requires analytical data which are comparable between laboratories and over time

As of May 2021, 36 U.S. states as well as Canada and various European countries have passed laws allowing cannabis to be used for medical applications or for recreational purposes.

Predictably, as more countries are becoming open to legalizing cannabis, regulations are slowly following suit to ensure adequate product safety and quality. However, cannabis is unique in that while it spans healthcare, pharma, consumer goods, and agricultural markets, the rules and regulations governing cannabis products are inconsistant between countries and even within the same country.

The other sectors mentionned have had regulatory frameworks and product standards in place for a long time, and most of those standards are consistent from one jurisdiction to another. Eventually the same will happen for cannabis. One thing is for sure, with these new changes on the legal status of marijuana worldwide, there has been drastic requirements for inspecting, monitoring, and evaluating whether cannabinoid products present potential risks to human health.

SiliCycle offers products to support this industry to produce cannabis extracts of highest purity

SAMPLE PREPARATION SEPARATION PURIFICATION DETECTION R&D

> SiliaPrep™ SPE Cartridges

> SiliaChrom® HPLC Columns

> SiliaMetS® Metal Scavengers

> SiliaSep™ Flash Cartridges

> SiliaBond® Organic Scavengers

> SiliaPlate™ TLC Plates

> SiliCycle R&D Services

 

Risk Assessment

There are various approaches to the assessment and management of hazards that can be applied to cannabis programs.

Inspired by the food industry and their Hazard Analysis and Critical Control Point (aka HACCP), the cannabis industry has created the Preventive Control Plan (PCP). The PCP is part of the GPP requirements for processors, and acts as the guideline for how hazards and risks are addressed to cannabis extracts, edible products or anything that will be used as an ingredient in either one. Hazards can be biological (ex: bacteria, viruses, molds), chemical (ex: food additives, solvents, allergens) or physical (ex: dirt, stones, insects, metal flakes).

Simply put it is important to understand what are the possible contaminants, the sources of such contaminants, the risk of contamination to products, the process steps or controls in place to minimize or eliminate such contamination as well as their control points, validation of measures to ensure effectiveness, and the responsible parties whom have access to the written plan.(1)

Adapted from Health Canada (2019). Good Production Practices Guide for Cannabis. Cannabis Regulations. 78-94.

Labs Challenges

Even though cannabis laboratories are maturing, they're maturing in an environment far different than labs from regulated industries, like food laboratories.

Food safety testing laboratories have been governmentally regulated and funded from almost the very beginning, allowing them some financial breathing room to set up their operation, and ensuring they won't be penalized for failing samples.

In contrast, testing fees for cannabis labs are paid by growers and producers – many of whom are just starting their own business and limited resources. This creates fierce competition between cannabis laboratories in terms of testing cost and turnaround time.

One similarity that the cannabis industry shares with the food industry is consumer and regulatory demand for safe products. This demand requires laboratories to invest in instrumentation and personnel to ensure generation of quality data. In short, the two major demands placed on cannabis laboratories are low cost and scientific excellence.

Scientific excellence isn't cheap, thus cannabis laboratories are stuck between a rock and a hard place and are feeling the squeeze.

Responding to the Challenges

There are three types of data collected, evaluated and combined in a risk assessment:

  • Sources/hazards such as: contaminants, pesticides, microbes or active ingredients.
  • Health effects/consequences/adverse events associated with each hazard
  • Exposure which involves sampling of products to determine concentrations of ingredients/contaminants and human exposure through use of the target product

SiliCycle offers a wide selection of analytical solutions for contaminant or ingredient data collection such as cannabinoids, terpenes, mycotoxins, heavy metals, pesticides, and residual solvents.

Various Contaminants to Consider

■ Pesticides

Selection of target pesticides for testing vary by state in the US. For example, Massachusetts' Medical Marijuana Program requires testing prohibited pesticides identified by the American Herbal Pharmacopoeia(2) which are commonly used in cannabis cultivation. But New Jersey's program selected pesticides for testing based on the EPA pesticide testing method 507.(3,4) As another example, Oregon Health Authority's technical report can be found online as a guide.(5)

In Canada, only certain pesticides have been approved for use on fresh cannabis, cannabis plants and dried cannabis, and their limits are federally regulated under Part 6 of the Cannabis Regulations.(6) This diversity of matrices complicates the task of analytical laboratories, which must adapt their sample preparation methods.

 

■ Solvents

Various solvents are used during the manufacturing of cannabis extracts and concentrates to remove cannabinoids from the plant material. For example, one of the most popular solvents used is ethanol which is present in the vast majority of processes at one time or another. Each solvent used has its own extraction efficiency, toxicity and latency within the extracted product. The compounds used for the extraction of cannabinoids may also pose a health risk.

The US Pharmacopeia's National Formulary (chapt. 467) provides guidance(7) for the use of solvents in the manufacturing of pharmaceutical products. This chapter has been adopted by many regulatory agencies in selecting solvents that may be utilized for extraction, as well as in setting the limits for residual solvents allowed in extracted products. However, some states have set their own limits such as Oregon, which has based their limits on the International Conference on Harmonized Tripartite Guideline, impurities: Guideline for Residual Solvents Q3C(R5) (ICHQ3C).(8)

In Canada, similarly to pesticides, the federal goverment has a list of limits for residual solvents to ensure product quality and safety is consistant throughout the country as whole.9

 

■ Microbiologicals & Mycotoxins

Typical Mycotoxins that may develop on cannabinoid crops.

A review of existing literature shows that the presence of mold on cannabis can cause severe health complications and, in certain cases, death. Pathogenic bacteria may also be a cause of under-reported or recognized adverse events.

For example, kidney failure can occur due to gastrointestinal infection linked to the smoking of cannabis which previously failed testing for the presence of enterobacteria and mold.

In general, bacteria cannot survive either the drying or heating processes to which cannabis is subjected. Salmonella, however, can survive at very low moisture levels and is highly infectious in humans. E. coli itself does not usually pose a significant health risk, but it is an indicator of poor sanitary conditions and the possible presence of other fecal bacteria.

As examples: Aspergillus genus has spores which can withstand desiccation and high temperatures, and can cause respiratory infections in individuals who inhale it if they are immune-compromised. There is a known clinical correlation with cannabis smoking. Aflatoxins, a family of toxins produced by fungi and which the aspergillus genus is part of, are highly carcinogenic mycotoxins which pose significant threat to exposed individuals.

 

■ Metals

A solution is purified from metallic impurities using scavengers

Cultivation of cannabis requires soil and water of a certain quality, i.e. free of contaminants. Since this might not always be the case, screening of heavy metals is recommended to safeguard the cannabis user's health. Heavy metals such as lead, cadmium, mercury, and arsenic are toxic to both plants and humans, and therefore often the focus of testing.

For purification means, our Metal & Organic Scavengers offer a powerful, quick and versatile solution at all scales and imaginable formats. They have rapidly become blockbusters in all sorts of purification processes.
> read more

 

■ Cannabinoids

Sugary crystals of a cannabis nugget

Potency of cannabis products may vary largely by strain.

The goal in determining what cannabinoids should be quantified is to support label accuracy. Although cannabis contains more than 150 cannabinoids, delta-9-tetrahydrocannabinol (Δ9-THC) has received the most attention since it is the principal psychoactive component of the plant.

Other analytes often required for analysis include cannabidiolic acid (CBD-A), cannabigerolic acid (CBGA), cannabidiol (CBD), cannibigerol (CBG), tetrahydrocannabinol acid (THCA), cannabinol (CBN) and delta-8-THC (Δ8-THC).

In addition, CBD must be analyzed for each product and indicated on the labels along with the THC mentioned above, the ACBD (cannabidiolic acid) and the ATHC (delta-9-tetrahydrocannabinolic acid).

 

Resources

(1) https://www.canada.ca/en/health-canada/services/cannabis-regulations-licensed-producers/good-production-practices-guide/guidance-document.html#appf

(2) AHP. 2013. Cannabis Inflorescence, Cannabis spp., Standards of Identity, Analysis, and Quality Control. American Herbal Pharmacopoeia 2013.
Available for purchase at: https://herbal-ahp.org/online-ordering-cannabis-inflorescence-qc-monograph/

(3) EPA. Method 507: Determination of Nitrogen- and Phosphorus-containing pesticides in water by gas chromotagraphy with a nitrogen-phosphorus detector. Revision 2.1. Edited by J.W. Munch (1995).
Available at https://www.cromlab.es/Articulos/Metodos/EPA/500/507.pdf

(4) EPA. Inert Ingredients Eligible for FIFRA 25(b) Pesticide Products (Updated December 2015).

Available at https://www.epa.gov/pesticide-registration/inert-ingredients-overview-and-guidance

(5) https://public.health.oregon.gov/PreventionWellness/marijuana/Documents/oha-8964-technical-report-marijuana-contaminant-testing.pdf

(6) https://www.canada.ca/en/public-health/services/publications/drugs-health-products/cannabis-testing-pesticide-list-limits.html

(7) https://www.pharmacopeia.cn/v29240/usp29nf24s0_c467.html

(8) https://www.pmda.go.jp/files/000156308.pdf

(9) https://www.canada.ca/en/health-canada/services/drugs-medication/cannabis/laws-regulations/regulations-support-cannabis-act/limits-residual-solvents.html

 

SiliCycle's Solutions Flow Chart

Cannabis analysis cannot be done with a simple and unique experiment.

Analytical labs first need to:

  • Prepare an effective sample for subsequent detection of the various compounds previously presented,
  • Detect, and then separate the latter for thorough analysis,
  • Purify the sample lot for delivery to market while minimizing loss of yield.

The schematic flow chart below presents at a glance SiliCycle's recommended products for each step of a comprehensive and exhaustive analysis.

As mentionned previously, laws and regulations in this industry vary between juridications and are consistantly changing. Therefore it is important to always check the current regulations in your area to see which treatments are allowed by law during the product transformation process.

 

SiliCycle: Purity at work!

■ Sample Preparation

Sample preparation is crucial for cannabis analysis due to two main reasons; it is a complex natural product and there is a wide variety of possible matrices (dry biomass, wet biomass, full spectrum extract, distillate, isolate,...) which each have their specificity (cannabinoid content, composition, state...). Given the wide range of physical properties of contaminants, both liquid chromatography (LC) and gas chromatography (GC) methods are required for testing, but this can only be acheived once an efficient sample preparation step has been done.

SiliaPrep™ SPE Cartridges

By using our products you will generate higher purity samples and reduce the number of false positives in your screening, resulting in higher quality data. All our SPE cartridges are packed with sorbents made of our fine-free SiliaFlash silica gel which has the highest purity on the market. When you use SiliCycle's SPE we guarantee the following:

  • High quality and wide variety of SiliaBond sorbents available
  • Excellent separation (very tight particle size distribution and no fines)
  • High recoveries and yields
  • No needle clogging
  • Less time and solvent spent conditioning the sorbent
  • No silica, plastic, or grease contamination of your final product
  • Lot-to-lot reproducible results

 

SiliCycle SPE Interference Removal Strategy

Special sorbent of choice is packed in a SPE cartridge:

  • Conditioning step: with six to ten hold-up volumes of solvent
  • Loading step: API is loaded and trapped onto the cartridge bed
  • Washing step: cartridge is washed to filter excess reagents and/or other impurities
  • Elution step: API is eluted and recovered

 

SiliCycle SPE cartridges formats are adaptable to all scales

We can provide a complete range of SPE cartridge lengths and diameters.

> learn more about SiliaPrep and SiliaPrepX SPE Cartridges

 

■ Separation

The rapid growth of the cannabis testing market has prompted the development of equally rapid methods to analyze the active ingredients.

SiliaChrom® HPLC Columns

SiliaChrom columns are made from extremely pure silicas and are well known for their high efficiency and resolution capacity. Based on spherical, totally porous silica, SiliaChrom columns provide enhanced chemical and mechanical stability as well as very high loading capacity.

All SiliaChrom columns are packed using our proprietary slurry packing process, to achieve a uniform column-to-column reproducibility.

SiliCycle has been manufacturing and packing HPLC columns for many years and offer more than 40 different phases. Raw materials and HPLC columns go through our ISO 9001-2008 registered manufacturing facility, under strict SOP's and standard QC column performance testing, assuring column performance, peak symmetry and lot-to-lot reproducibility.

The SiliaChrom portfolio ranges from reversed-phase to normal phase columns, columns for large proteins and peptide analysis and SFC compatible solutions. An incredibly range of column dimensions and particle sizes are available to accommodate the vast majority of your applications.

SiliaChrom HPLC Columns Characteristics

Main Characteristics SiliaChrom Phases Particle Size (μm) Pore Size (Å) Specific Surface Area (m2/g)
  • Wide range of selectivities
  • Ultra-pure metal-free silica (99.9999 % purity)
  • High column performance and resolution
  • Enhanced batch-to-batch reproducibility
  • Extended column lifetime
  • Reduced silanol activity, better peak symmetry
  • Extremely low bleeding for LC-MS applications
  • Easy scale-up to preparative formats
Plus C18 3, 5, 10 100 370 - 430
Plus C18-300 3, 5, 10 300 80 - 120
Plus C8 3, 5, 10 100 370 - 430
Plus C8-300 3, 5, 10 300 80 - 120
Plus C4 3, 5, 10 100 370 - 430
Plus C4-300 3, 5, 10 300 80 - 120
Plus PFP 3, 5, 10 120 320 - 360
Plus Phenyl 3, 5, 10 100 370 - 430
Plus Cyano 3, 5, 10 100 370 - 430
Plus Amino 3, 5, 10 100 370 - 430
Plus Diol 3, 5, 10 100 370 - 430
Plus Silica 3, 5, 10 100 370 - 430
Plus SAX 3, 5, 10 Proprietary Information
Plus SCX 3, 5 Proprietary Information
  • Stable from 100 % aqueous to 100 % organic
  • Enhanced retention of hydrophilic molecules
  • Inertness for acidic and basic analytes
dt C18 2.5, 3, 5, 10 100 410 - 440

> learn more about SiliaChrom HPLC Columns

 

■ Purification

SiliaMetS E-PAK® – Radial Fixed Bed Flow-Through Cartridges

Created with proprietary technology, E-PAK cartridges provide rapid adsorption kinetics at flow rates and processing capacities suitable for laboratory, pilot and commercial operations.

Features & Benefits
  • Proven cartridge design ensures rapid, simple & reliable technology
  • High adsorption capacity and flow rate
  • Fixed-bed design ensuring safer handling, clean-up and disposal
  • Large adsorbent capacity in small area footprint increases product recovery & reduces solvent requirements
Sorbents

Active Adsorbents Impurity Removed and/or Recovered
SiliaMetS Amine, Diamine and Triamine Best for: Pd, Cr, Pt, W, Zn
Good for: Cd, Co, Cu, Fe, Hg, Ni, Pb, Ru, Sc & Se
SiliaMetS AMPA Best for: Al, Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Mn, Nd, Ni, Pm, Pr, Sb, Sn, Tb, Tm, V, Yb
Good for: Co, Cu, Fe, Mg & Zn
SiliaMetS DMT Best for: Pd, As, Ir, Ni, Os, Pt, Rh, Ru, Se
Good for: Cd, Co, Cu, Fe, Sc & Zn
SiliaMetS Imidazole Best for: Cd, Co, Cu, Fe, Ir, Li, Mg, Ni, Os, W, Zn
Good for: Cr, Pd & Rh
SiliaMetS TAAcOH Best for: Ca, Co, Ir, Li, Mg, Ni, Os, Ru, Sc
Good for: Cr, Cs, Fe, Pd, Rh & Sn
SiliaMetS TAAcONa Best for: Ca, Cd, Cs, Cu, Fe, Ir, La, Li, Mg, Ni, Os, Rh, Sc, Sn
Good for: Cr, Pd, Ru, Se & Zn
SiliaMetS Thiol Best for: Pd, Ag, Hg, Os, Ru
Good for: Cu, Ir, Pb, Rh, Se & Sn
SiliaFlash Bare Silica Very vast range of organic impurities, metals, pigments, etc.
SiliaBond Cyano & Florisil® Various organic molecules
SiliaBond Propylsulfonic Acid (SCX-2) Amines & Anilines, Ion Exchange
SiliaCarb VW, VA, HA and CA Precious metal catalysts, pigments and reaction contaminants

Lab Scale Purification

Cartridge Size Flow Rate Range* SiliaMetS & SiliaBond Weight SiliaFlash & Activated Carbons Weight
5 x 1 cm 1 - 20 mL/min 8 g 5 g
5 x 10 cm 10 - 200 mL/min 75 g 50 g
5 x 25 cm 25 - 500 mL/min 200 g 125 g

* Faster flow rate can be used for the lab scale cartridges depending on the application or the scavenging difficulty (1 cm up to 100 mL/min, 10 cm up to 500 mL/min and 25 cm up to 1 L/min).

Pilot and Commercial Scale Purification

Purification Scale Cartridge Size Flow Rate Range SiliaMetS & SiliaBond Weight SiliaFlash & Activated Carbons Weight
Pilot Scale 16.5 x 12.5 cm 0.10 - 2.5 L/min 875 g 850 g
16.5 x 25 cm 0.25 - 5 L/min 1.75 kg 1.7 kg
Commercial Scale 16.5 x 50 cm 0.50 - 10 L/min 3.5 kg 3.4 kg
16.5 x 100 cm 1 - 20 L/min 7 kg 6.8 kg

> learn more about E-PAK Purification Cartridges

 

SiliaSep™ Flash Cartridges

Silica is the most widely used matrix in chromatography.

These bare and grafted supports possess great properties for uses as stationary phases and are particularly appreciated for their high mechanical resistance. We offer the largest range of functionalized silicas, available with capped or uncapped residual silanol groups.

The use of SiliaSep Flash cartridges improves purification efficiency by offering superior reproducibility and productivity compared to conventional manual flash chromatography.

> learn more about SiliaSep Flash Cartridges

 

SiliaFlash® & SiliaSphere® PC Bulk Silica Gels

All our SPE & Flash cartridges phases are available in bulk as well, so you can do your own packing in the format that best suits your application or routine.

SiliaFlash irregular gel and SiliaSphere spherical gel are available from g to multi tons, both as bare or functionalizes silicas, in various particle and pore sizes.

For easy and simple separation, our blockbuster is a 40 - 63 μm, 60 Å gel. We name it R12030B.

For trickier separation, spherical particles are ideal, and S10030B-A is R12030B equivalent in terms of particle / pore size.

> learn more about SiliaFlash Bulk Irregular Silica Gels

> learn more about SiliaSphere Bulk Spherical Silica Gels

 

■ Detection

Because there is more than just analysis.

Purification of your sample is your final aim, and we will be your best partner for all kind of purification issues and scales.

SiliaPlate™ TLC Plates

Thin layer chromatography (TLC) is a quick, simple and inexpensive analytical technique frequently used in various laboratories as it is one of the most verstatile. It is used for:

  • Reaction Monitoring
  • Screening
  • Compound purity evaluation

Rapid and cost-efficient selection and optimization of chromatographic conditions prior to flash chromatography purification or HPLC analysis.

Besides speed and low cost, TLC analysis presents other advantages like small quantity of compound required and high sample throughput capability (up to 20 samples simultaneously).

SiliaPlate represents an efficient and economical alternative to other TLC plate manufacturers while demonstrating high separation power, which is due to our narrow particle size distribution silica gel used for manufacturing.

SiliaPlate Available Chemistries

Reversed-Phases Normal Phases

C18 (Si-C18)
(TLX-R30414BK-XXX)

C8 (Si-C8)
(TLX-R31014BK-XXX)

C2 (Si-C2)
(TLX-R32614BK-XXX)

Silver Nitrate (Si-AGNO3) 10, 15 or 20 %
(TLX-R32X14BK-XXX)

Bare Silica (Si)
(TLX-R10014BK-XXX)

Amine (Si-WAX)
(TLX-R52014BK-XXX)

Cyano (Si-CN)
(TLX-R38014BK-XXX)

Diol (Si-Diol)
(TLX-R35014BK-XXX)

Aluminum Oxide
(TLX-AUT0337-XXX)

SiliaPlate Available Backings
  • Glass (TLG-RXX14BK-XXX)
  • Aluminum (TLA-RXX11B-XXX)
  • Plastic (TLP-RXX11B-XXX)
SiliaPlate Available Plate Sizes
  • 2.5 x 5 cm
  • 2.5 x 7.5 cm
  • 2.5 x 10 cm
  • 4 x 8 cm
  • 5 x 6.7 cm
  • 5 x 7.5 cm
  • 5 x 10 cm
  • 5 x 20 cm
  • 10 x 10 cm
  • 10 x 20 cm
  • 20 x 20 cm
SiliaPlate Available Backings
  • Scored Plates
  • Channeled Plates
  • Preparative Plates
  • High Performance Plates
  • Thicknesses from 100 to 2,000 μm

> learn more about SiliaPlate TLC Plates

 

SiliaMetS Metal Scavengers & SiliaBond Organic Scavengers

SiliCycle grafted technology enables more powerful purification processes to help reach new purity standards. Our solutions are extremely versatile and customizable.

Because it's not enough just to identify and quantify,
Because you don't need to waste a given lot just by reason of too many impurities,
This is when our scavengers come to the rescue

  • SiliaMetS are functionalized silica that will scavenge various types of metals (we pretty much have functionalities for almost all metals & metallic complexes).
  • SiliaBond are functionalized silica that will scavenge various types of organic residues (we pretty much have functionalities for almost all organic functionalities).

Easier, Cleaner, Faster, Efficient Purification Processes

  • Almost two decades of know-how in silica-grafting and scavenging technology
  • Broadest portfolio of scavengers with associated applications: agrochemicals, mining, fine chemicals, water and waste treatment
  • Great compatibility with a myriad of experimental conditions, solvents, pH and temperatures
  • Strong chemical, physical, thermal and mechanical stability

How Will Scavengers Help You Clean Your Sample?

Because we all know images speak more that words:

> learn more about SiliCycle's Scavenging Solutions

 

SiliCycle R&D Services

Need help to develop your purification method for the highest cannabis purity on the market ?

We'll help you. Reinvesting our experts' talent in your own expertise is what drives our passion

For any issue you may have, we offer high-throughput R&D services.

  • We listen. We understand. We work with you.
  • Assistance to start-ups & young tech companies.
  • We are flexible, commited, reliable, innovative, fast & affordable.

Our Scientific Team Expertise & Talents

Scientific Team & Know-How

SiliCycle's mandate is to offer on-time tailored packages of work with communication report format, cost and timeframe in line with your projects.

Our domain of expertise lies in our experts' vast knowledge and skills in a variety of core competencies in various domains. SiliCycle's team of in-house experts ensures that every project comes with an original and flexible solution that matches your needs.

A Brief Overview of Our Scientists' Competencies

  • Analytical Chemistry
    • Analytical method development and optimization (UPLC, HPLC, GC, etc.)
    • Extraction of natural compounds
    • Sample preparation using various techniques (SPE, etc.)
    • Method validation under Good Laboratories Practices norms

... as well as a vast experiences in other spheres of competence such as:

  • Medicinal & Organic Chemistry
  • Biology, Biochemistry
  • Catalysis & Organometallic Chemistry
  • Chemical Engineering, Mesostructured Material, Physical & Petrochemistry

> learn more about SiliCycle R&D Services