Growing Analytical Solutions For Cannabis Testing

Innovative Products And Expertise For Fast, Accurate, Reliable Results

We get it. Your market is quickly changing and you need a chromatography partner that understands that. Whether you are part of a well-established safety and potency lab or starting a new lab, Restek has the products and expertise you need for successful cannabis analyses. Being an employee-owned and independent chromatography company, every employee at Restek has a vested interest in your success. We design the best solutions for your lab, regardless of the instrumentation and techniques used. Here, you will find innovative LC and GC products and methodologies designed to fit your toughest analytical problems.

We’ve been in your shoes. That’s why we understand your challenges and focus on solving them. Using our expertise to develop innovative products that help chromatographers has always been, and continues to be, Restek’s top priority. We strive to develop industry-leading technologies that fit the needs of today’s analysts. When setting up a laboratory for cannabis testing, we realize that you need dependable products that deliver high-quality data without considerable capital investment. We know you need to work with a company that understands the challenges of your market and supports you with tailored solutions and superior customer service.

PRODUCT POTENCY TESTING

Our High-Throughput LC and GC Cannabinoids Methods Produce Results Quickly without the Cost of New Equipment

When setting up a lab, often you just can’t invest in the latest instrumentation, but you still need to get results fast. We understand that. That’s why Restek has developed both LC and GC methods for cannabinoids that let you report potency results quickly. For LC, we created a fast analysis of 16 cannabinoids that can be performed on any LC instrument. By utilizing Raptor column technology, as shown in Figure 1, we developed a nine-minute analysis that is compatible with any HPLC instrument—so you get UHPLC speed on your existing equipment without the capital investment. Also, we specifically chose an easy-to-make mobile phase that can be directly transferred to LC-MS, if you ever need to move to MS due to regulation changes. For labs using GC equipment, you can analyze cannabinoids in just minutes using an Rxi-35Sil MS column and the instrument conditions shown in Figure 2. Why did we focus on fast cannabinoid analyses? Potency testing is the cornerstone of your lab. Building a fast method means your productivity increases and you can analyze more samples per day on the same instrument, delaying the need for expensive capital investments in new equipment.

Figure 1: Raptor LC columns give you fast analysis times for cannabinoids without the expense of UHPLC equipment.

Peaks tR (min) 1. Cannabidivarinic acid (CBDVA) 1.877 2. Cannabidivarin (CBDV) 2.086 3. Cannabidiolic acid (CBDA) 2.592 4. Cannabigerolic acid (CBGA) 2.750 5. Cannabigerol (CBG) 2.912 6. Cannabidiol (CBD) 3.084 7. Tetrahydrocannabivarin (THCV) 3.391 8. Tetrahydrocannabivarinic acid (THCVA) 4.279 Peaks tR (min) 9. Cannabinol (CBN) 4.609 10. Cannabinolic acid (CBNA) 5.437 11. Δ9-Tetrahydrocannabinol (Δ9-THC) 5.815 12. Δ8-Tetrahydrocannabinol (Δ8-THC) 6.002 13. Cannabicyclol (CBL) 6.916 14. Cannabichromene (CBC) 7.263 15. Tetrahydrocannabinolic acid A (THCA-A) 7.612 16. Cannabichromenic acid (CBCA) 8.510 LC_GN0578 Column Raptor ARC-18 (cat.# 9314A65) Dimensions: 150 mm x 4.6 mm ID Particle Size: 2.7 µm Pore Size: 90 Å Guard Column: Raptor ARC-18 EXP guard column cartridge 2.7 µm (cat.# 9314A0250) Temp.: 30 °C Sample Tetrahydrocannabivarin (cat.# 34100) Cannabidiolic acid (CBDA) (cat.# 34094) Cannabichromene (CBC) (cat.# 34092) Cannabigerol (CBG) (cat.# 34091) delta-9-Tetrahydrocannabinolic acid A (THCA-A) (cat.# 34093) delta-8-Tetrahydrocannabinol (Δ8-THC) (cat.# 34090) delta-9-Tetrahydrocannabinol (Δ9-THC) (cat.# 34067) Cannabinol (CBN) (cat.# 34010) Cannabidiol (CBD) (cat.# 34011) Compounds not present in these mixes were obtained separately. Diluent: 25:75 Water:methanol Conc.: 50 µg/mL Inj. Vol.: 5 µL Mobile Phase A: Water, 5 mM ammonium formate, 0.1% formic acid B: Acetonitrile, 0.1% formic acid Time (min) Flow (mL/min) %A %B 0.00 1.5 25 75 9.00 1.5 25 75 Detector UV/Vis @ 228 nm Instrument HPLC

Figure 2: Determine critical cannabinoids in minutes by GC using an Rxi-35Sil MS column.

Peaks Conc. (µg/mL) tR (sec) 1. Phencyclidine (IS) 50 73.4 2. Cannabidivarin 100 115.2 3. Tetrahydrocannabivarin 100 130.3 4. Cannabichromene 100 138.3 5. Cannabidiol 100 150.0 6. Δ8-Tetrahydrocannabinol 100 152.1 7. Δ9-Tetrahydrocannabinol 100 156.1 8. Cannabigerol 100 159.5 9. Cannabinol 100 165.6 10. Prazepam (IS) 50 192.4 GC_FS0549 Column Rxi-35Sil MS, 15 m, 0.25 mm ID, 0.25 µm (cat.# 13820) Sample Phencyclidine (cat.# 34027) Cannabichromene (CBC) (cat.# 34092) Cannabinoids standard (cat.# 34014) delta-8-Tetrahydrocannabinol (THC) (cat.# 34090) Cannabigerol (CBG) (cat.# 34091) Prazepam (cat.# 34055) Injection Inj. Vol.: 1 µL split (split ratio 20:1) Liner: Premium 4 mm Precision liner w/wool (cat.# 23305.5) Inj. Temp.: 250 °C Oven Oven Temp.: 190 °C (hold 0.1 min) to 330 °C at 35 °C/min (hold 0.9 min) Carrier Gas H2, constant flow Flow Rate: 2.5 mL/min Detector FID @ 350 °C Constant Column + Constant Make-up: 50 mL/min Make-up Gas Type: N2 Hydrogen flow: 40 mL/min Air flow: 450 mL/min Data Rate: 20 Hz Instrument Agilent/HP6890 GC Notes Cannabidivarin and tetrahydrocannabivarin standards were obtained from BOC Sciences.

TERPENE PROFILING

Reduce Capital Investments—Analyze Terpenes by GC on the Same Setup Used for Residual Solvents

Cannabis has a complex terpene profile, which is theorized to increase its therapeutic effects. Terpene profiling is used for both product quality testing and strain identification. These complex and sometimes problematic compounds are challenging to analyze, but the experts at Restek have developed qualitative GC methodology for terpene profiling that fits easily into required laboratory workflows. To keep things simple, the GC terpene profile analysis in Figure 3 can be performed on the same instrument and column that we recommend for residual solvent testing.

Figure 3: Comprehensive terpene analysis by headspace GC-FID can be done on the same instrument and GC column as residual solvents analysis, which simplifies setup and improves lab productivity.

Peaks tR (min) 1. α-Pinene 7.39 2. Camphene 7.71 3. β-Myrcene 7.98 4. Sabinene 8.02 5. β-Pinene 8.11 6. α-Phellandrene 8.4 7. δ 3-Carene 8.44 8. α-Terpinene 8.57 9. Ocimene 8.61 10. Limonene 8.71 11. p-Cymene 8.75 12. β-Ocimene 8.82 13. Eucalyptol 8.91 14. γ-Terpinene 9.06 15. Terpinolene 9.47 16. Linalool 9.87 17. Fenchone 10.06 18. Isopulegol 10.73 Peaks tR (min) 19. dl-Menthol 11.08 20. Borneol 11.19 21. α-Terpineol 11.29 22. Dihydrocarveol 11.40 23. Citronellol 11.51 24. Geraniol 11.82 25. 2-Piperidinone 11.88 26. Citral 1 11.92 27. Pulegone 11.97 28. Citral 2 12.24 29. Citral 3 13.19 30. Citral 4 13.43 31. β-caryophyllene 13.83 32. α-Humulene 14.21 33. Nerolidol 1 14.78 34. Nerolidol 2 15.08 35. Caryophyllene oxide 15.92 36. α-Bisabolol 16.43 GC_FS0518 Column Rxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868) Sample Terpenes mix Diluent: Isopropyl alcohol Conc.: 200 ng/µL (0.02% wt/vol). The sample was prepared by placing 10 µL into the headspace vial. Injection headspace-loop split (split ratio 10:1) Liner: Premium 1.0 mm ID straight inlet liner (cat.# 23333.1) Headspace-Loop Inj. Port Temp.: 250 °C Instrument: Tekmar HT-3 Inj. Time: 1.0 min Transfer Line Temp.: 160 °C Valve Oven Temp.: 160 °C Needle Temp.: 140 °C Sample Temp.: 140 °C Sample Equil. Time: 30.0 min Vial Pressure: 20 psi Loop Pressure: 15 psi Oven Oven Temp.: 60 °C (hold 0.10 min) to 300 °C at 12.50 °C/min (hold 3.0 min) Carrier Gas He, constant flow Linear Velocity: 33 cm/sec Detector FID @ 320 °C Make-up Gas Flow Rate: 45 mL/min Make-up Gas Type: N2 Hydrogen flow: 40 mL/min Air flow: 450 mL/min Data Rate: 20 Hz Instrument Agilent/HP6890 GC Notes For qualitative purposes only.

RESIDUAL SOLVENT ANALYSIS

Improve Productivity—Keep Analyzing Samples Instead of Changing Columns between Residual Solvent and Terpene Methods.

As the popularity of cannabis grows, so does concern over the safety of the drug products. Cannabis concentrates can contain residual solvents left over from manufacturing that can be harmful to human health. Because of this risk, many states will require residual solvent testing of cannabis concentrates. Due to their high volatility, residual solvents can only be analyzed using GC techniques. The chemists at Restek have developed a quick and easy method that allows for residual solvent analysis (Figure 4) and terpene profiling (Figure 3) on the same column and instrument platform with minimal sample preparation.

Figure 4: Improve productivity and reduce downtime for column changes—this sensitive headspace GC-FID analysis of residual solvents can be accomplished on the same instrument and Rxi-624Sil MS column that is used in Restek’s terpenes profiling method.

Peaks tR (min) Conc. (µg/mL) 1. n-Propane 1.492 10 2. Isobutane 1.708 10 3. n-Butane 1.901 10 4. Methanol 2.215 10 5. n-Pentane 3.018 10 6. Ethanol 3.212 10 7. Diethyl ether 3.344 10 8. Acetone 3.820 10 9. 2-Propanol 4.188 10 10. Acetonitrile 4.367 10 11. Methylene chloride 4.710 10 12. n-Hexane 6.033 10 13. Ethyl acetate 7.675 10 14. Chloroform 8.104 10 15. Cyclohexane 8.328 10 16. Benzene 8.763 10 17. 1,2-Dichloroethane 8.872 10 18. n-Heptane 9.236 10 19. Trichloroethene 9.637 10 20. Toluene 11.500 10 21. m-Xylene 13.421 10 22. p-Xylene 13.421 10 23. o-Xylene 13.725 10 24. N,N-Dimethylacetamide (solvent) 13.958 GC_GN1198 Column Rxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868) Sample Residual solvents #1 (cat.# 34105) n-Propane, isobutane, n-butane (Emerald Scientific) Diluent: N,N-Dimethylacetamide Conc.: 10 µg/mL Injection Inj. Vol.: 250 µL headspace-syringe split (split ratio 10:1) Liner: Topaz 1.8 mm ID straight/SPME inlet liner (cat.# 23280) Inj. Temp.: 280 °C Headspace-Syringe Split Vent Flow Rate: 20 mL/min Instrument: PAL RTC Syringe Temp.: 150 °C Sample Temp.: 80 °C Sample Equil. Time: 45 min Inj. Speed: 1700 µL/sec Oven Oven Temp.: 30 °C (hold 6 min) to 85 °C at 15 °C/min (hold 2 min) to 250 °C at 35 °C/min Carrier Gas He, constant flow Flow Rate: 2 mL/min Linear Velocity: 40.63 cm/sec Detector FID @ 320 °C Make-up Gas Flow Rate: 40 mL/min Make-up Gas Type: N2 Hydrogen flow: 45 mL/min Air flow: 450 mL/min Data Rate: 20 Hz Instrument Agilent 7890B GC

Pesticide Analysis

Ensure Product Safety with Fast, Selective Multiresidue Pesticide Analysis

In addition to residual solvents, cannabis products can contain residues of pesticides that were applied to cannabis plants during growth in order to control agricultural pests. These pesticides can be analyzed by LC-MS/MS, GC-MS/MS, and GC-MS. Regardless of the technique used, lists of target compounds can be extensive, so column selectivity is an important factor in achieving good separations. Both Raptor ARC-18 LC columns (Figure 5) and Rxi-5ms GC columns (Figure 6) provide the selectivity needed for accurate and reliable multiresidue pesticides analysis. Removing matrix interferences while also recovering the analytes of interest is also crucial for a successful pesticide analysis using either LC or GC, and Restek’s Q-sep QuEChERS products allow for fast, easy, adaptable cleanup of a wide variety of matrices.

Figure 5: A high-throughput separation of 204 pesticides by LC-MS/MS can be achieved in only 7 minutes with the Raptor ARC-18 column.
View peak list
LC_FF0541 Column Raptor™ ARC-18 (cat.# 9314A12) Dimensions: 100 mm x 2.1 mm ID Particle Size: 2.7 µm Temp.: 50 °C Sample LC multiresidue pesticide kit (cat.# 31971) Diluent: Water Conc.: 20 ng/mL Inj. Vol.: 5 µL Mobile Phase A: Water + 2 mM ammonium formate + 0.2% formic acid B: Methanol + 2 mM ammonium formate + 0.2% formic acid Time (min) Flow (mL/min) %A %B 0.00 0.4 95 5 2.00 0.4 40 60 4.00 0.4 25 75 6.00 0.4 0 100 7.00 0.4 0 100 7.01 0.4 95 5 9.50 0.4 95 5 Max Pressure: 525 bar Detector Waters Xevo TQ-S Ion Source: Waters Zspray™ ESI Ion Mode: ESI+ Mode: MRM Instrument Waters ACQUITY UPLC I-Class Notes When combining a large number of compounds with different chemical functionalities, mix stability can be an issue. In formulating our LC multiresidue pesticide standard kit (cat.# 31971), we extensively studied the 204 compounds involved, then grouped them into as few mixes as possible while still ensuring maximum long-term stability and reliability. Several of these compounds are isomeric and separation of the isomers accounts for 216 peaks in the chromatogram compound list. For quantitative analysis, we recommend analyzing each mix separately to ensure accurate results for every compound.

Figure 6: Rxi-5ms GC columns reliably separate many commonly used pesticides.

Peaks tR (min) 1. Tefluthrin 14.23 2. Transfluthrin 15.18 3. Anthraquinone 16.02 4. Bioallethrin 17.17 5. Resmethrin 1* 20.43 6. Resmethrin 2* 20.55 7. Tetramethrin 1* 21.00 8. Tetramethrin 2* 21.14 9. Bifenthrin 21.15 10. Phenothrin 1* 21.59 11. Phenothrin 2* 21.71 12. lambda-Cyhalothrin 22.30 13. Acrinathrin 22.51 14. cis-Permethrin 23.14 15. trans-Permethrin 23.29 Peaks tR (min) 16. Cyfluthrin 1* 23.83 17. Cyfluthrin 2* 23.93 18. Cyfluthrin 3* 24.02 19. Cyfluthrin 4* 24.06 20. Cypermethrin 1* 24.19 21. Cypermethrin 2* 24.30 22. Cypermethrin 3* 24.39 23. Cypermethrin 4* 24.43 24. Flucythrinate 1* 24.43 25. Flucythrinate 2* 24.66 26. Fenvalerate 1* 25.25 27. tau-Fluvalinate 1* 25.47 28. Fenvalerate 2* 25.48 29. tau-Fluvalinate 2* 25.53 30. Deltamethrin 26.09 *Isomers numbered according to elution order. GC_FS0605 Column Rxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423) Sample GC multiresidue pesticide standard #6-SPP (cat.# 32568) Diluent: Toluene Conc.: 100 µg/mL Injection Inj. Vol.: 1 µL split (split ratio 50:1) Liner: Premium 4.0 mm ID Precision inlet liner w/wool (cat.# 23305.1) Inj. Temp.: 250 °C Oven Oven Temp.: 90 °C (hold 1 min) to 330 °C at 8.5 °C/min (hold 5 min) Carrier Gas He, constant flow Flow Rate: 1.4 mL/min Detector MS Mode: Scan Scan Program: Group Start Time (min) Scan Range (amu) Scan Rate (scans/sec) 1 5 55-550 7 Transfer Line Temp.: 290 °C Analyzer Type: Quadrupole Source Temp.: 325 °C Electron Energy: 70 eV Solvent Delay Time: 5 min Ionization Mode: EI Instrument Thermo Scientific TSQ 8000 Triple Quadrupole GC-MS Notes Bioallethrin isomers are only slightly resolved with this method, so they are treated as one peak. Reconstructed chromatogram from select ions.

By Breaking Boundaries in Our Industry, We Help You Succeed in Yours

Restek has been helping cannabis labs establish innovative, cost-effective analytical solutions from the very beginning, and we will continue to help you manage your ever changing analytical challenges every step of the way.