share:
delim
Article
article_image

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. We also offer a similar 35-type stationary phase on metal MXT tubing for labs using SRI GC instruments. 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.

PeakstR (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
PeakstR (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
16 Cannabinoids on Raptor ARC-18 2.7 μm by LC-UV
LC_GN0578
ColumnRaptor 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
SampleTetrahydrocannabivarin (cat.# 34100)
Cannabidiolic acid (CBDA) (cat.# 34099)
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
0.001.52575
9.001.52575
DetectorUV/Vis @ 228 nm
InstrumentHPLC

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

PeaksConc.
(µg/mL)
tR (sec)
1.Phencyclidine (IS)5073.4
2.Cannabidivarin100115.2
3.Tetrahydrocannabivarin100130.3
4.Cannabichromene100138.3
5.Cannabidiol100150.0
6.Δ8-Tetrahydrocannabinol100152.1
7.Δ9-Tetrahydrocannabinol100156.1
8.Cannabigerol100159.5
9.Cannabinol100165.6
10.Prazepam (IS)50192.4
Medical Cannabis Cannabinoids and Internal Standards on Rxi-35Sil MS
GC_FS0549
ColumnRxi-35Sil MS, 15 m, 0.25 mm ID, 0.25 µm (cat.# 13820)
SamplePhencyclidine (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 GasH2, constant flow
Flow Rate:2.5 mL/min
DetectorFID @ 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
InstrumentAgilent/HP6890 GC
NotesCannabidivarin and tetrahydrocannabivarin standards were obtained from BOC Sciences.

TECH TIP

Using Thomson SINGLE StEP filter vials is an ideal way to remove particulate matter that could clog your column.

They provide sample filtration that’s economical, eco-friendly, and fast!

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.

PeakstR (min)
1.α-Pinene7.39
2.Camphene7.71
3.β-Myrcene7.98
4.Sabinene8.02
5.β-Pinene8.11
6.α-Phellandrene8.4
7.δ 3-Carene8.44
8.α-Terpinene8.57
9.Ocimene8.61
10.Limonene8.71
11.p-Cymene8.75
12.β-Ocimene8.82
13.Eucalyptol8.91
14.γ-Terpinene9.06
15.Terpinolene9.47
16.Linalool9.87
17.Fenchone10.06
18.Isopulegol10.73
PeakstR (min)
19.dl-Menthol11.08
20.Borneol11.19
21.α-Terpineol11.29
22.Dihydrocarveol11.40
23.Citronellol11.51
24.Geraniol11.82
25.2-Piperidinone11.88
26.Citral 111.92
27.Pulegone11.97
28.Citral 212.24
29.Citral 313.19
30.Citral 413.43
31.β-caryophyllene13.83
32.α-Humulene14.21
33.Nerolidol 114.78
34.Nerolidol 215.08
35.Caryophyllene oxide15.92
36.α-Bisabolol16.43
Cannabis Terpenes on Rxi-624Sil MS by FET-HS-GC
GC_FS0518
ColumnRxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
SampleTerpenes mix
Diluent:Isopropyl alcohol
Conc.:200 ng/µL (0.02% wt/vol). The sample was prepared by placing 10 µL into the headspace vial.
Injectionheadspace-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 GasHe, constant flow
Linear Velocity:33 cm/sec
DetectorFID @ 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
InstrumentAgilent/HP6890 GC
NotesFor qualitative purposes only.

TECH TIP

Did you know that headspace analysis eliminates the possibility of column contamination from nonvolatile matrix components? This results in an extremely clean chromatogram, minimal instrument maintenance, and longer column lifetimes.

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.

PeakstR (min)Conc.
(µg/mL)
1.Propane1.1410
2.Isobutane1.3010
3.n-Butane1.4510
4.Methanol1.6910
5.n-Pentane2.3010
6.Ethanol2.4510
7.Acetone2.9110
8.Isopropanol3.1910
9.Acetonitrile3.3110
10.n-Hexane4.2310
11.Tetrahydrofuran5.2910
12.Chloroform5.6910
13.Carbon tetrachloride5.7010
14.Benzene5.9110
15.n-Heptane6.2510
16.Toluene8.0310
17.m-Xylene10.0610
18.p-Xylene10.0610
19.o-Xylene10.3910
20.Solvent (N,N-dimethylacetamide [DMA])10.64
Residual Solvents on Rxi-624Sil MS via HS-Syringe-GC-HES-MS
GC_GN1197
ColumnRxi-624Sil MS, 30 m, 0.25 mm ID, 1.40 µm (cat.# 13868)
Sample
Diluent:RO water
Conc.:10 µg/mL
Injection
Inj. Vol.:500 µL headspace-syringe split (split ratio 100:1)
Liner:Topaz 0.75 mm ID straight/SPME inlet liner (cat.# 23434)
Inj. Temp.:280 °C
Headspace-Syringe
Split Vent Flow Rate:3 mL/min
Instrument:PAL RTC
Syringe Temp.:135 °C
Sample Temp.:85 °C
Sample Equil. Time:2 min
Inj. Speed:500 µL/sec
Oven
Oven Temp.:30 °C (hold 3 min) to 85 °C at 15 °C/min (hold 2 min) to 250 °C at 35 °C/min (hold 2 min)
Carrier GasHe, constant flow
Flow Rate:2.0 mL/min
Linear Velocity:51 cm/sec
DetectorHES-MS
Scan Program:
GroupStart Time
(min)
Scan Range
(amu)
Scan Rate
(scans/sec)
1029-4506.4
Transfer Line Temp.:280 °C
Analyzer Type:Quadrupole
Source Type:HES
Aperture Size:6 mm ID
Source Temp.:350 °C
Quad Temp.:200 °C
Electron Energy:70 eV
Solvent Delay Time:0 min
Tune Type:PFTBA
Ionization Mode:EI
InstrumentAgilent 7890B GC & 5977B MSD

TECH TIP

You’ll save money ordering from Restek because we understand the need to control costs and build efficient workflows. We develop as many analyses as possible using the same columns and consumables, so you can minimize the number of products you need to stock.

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 Multiresidue Pesticide Standard Kit on Raptor™ ARC-18 by LC-MS/MS
LC_FF0541
ColumnRaptor™ ARC-18 (cat.# 9314A12)
Dimensions:100 mm x 2.1 mm ID
Particle Size:2.7 µm
Temp.:50 °C
SampleLC 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
0.000.4955
2.000.44060
4.000.42575
6.000.40100
7.000.40100
7.010.4955
9.500.4955
Max Pressure:525 bar
DetectorWaters Xevo TQ-S
Ion Source:Waters Zspray™ ESI
Ion Mode:ESI+
Mode:MRM
InstrumentWaters ACQUITY UPLC I-Class
NotesWhen 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.

PeakstR (min)
1.Tefluthrin14.23
2.Transfluthrin15.18
3.Anthraquinone16.02
4.Bioallethrin17.17
5.Resmethrin 1*20.43
6.Resmethrin 2*20.55
7.Tetramethrin 1*21.00
8.Tetramethrin 2*21.14
9.Bifenthrin21.15
10.Phenothrin 1*21.59
11.Phenothrin 2*21.71
12.lambda-Cyhalothrin22.30
13.Acrinathrin22.51
14.cis-Permethrin23.14
15.trans-Permethrin23.29
PeakstR (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.Deltamethrin26.09
*Isomers numbered according to elution order.
GC Multiresidue Pesticide Standard #6-SPP on Rxi-5ms by GC-MS
GC_FS0605
ColumnRxi-5ms, 30 m, 0.25 mm ID, 0.25 µm (cat.# 13423)
SampleGC 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 GasHe, constant flow
Flow Rate:1.4 mL/min
DetectorMS
Mode:Scan
Scan Program:
GroupStart Time
(min)
Scan Range
(amu)
Scan Rate
(scans/sec)
1555-5507
Transfer Line Temp.:290 °C
Analyzer Type:Quadrupole
Source Temp.:325 °C
Electron Energy:70 eV
Solvent Delay Time:5 min
Ionization Mode:EI
InstrumentThermo Scientific TSQ 8000 Triple Quadrupole GC-MS
NotesBioallethrin isomers are only slightly resolved with this method, so they are treated as one peak.

Reconstructed chromatogram from select ions.

TECH TIP

Struggling with matrix interferences or high backpressures? Contact Restek’s Technical Service team for guard column recommendations.

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.

Restek Domestic Customer Service

Subject

Message

Your Full Name

Your Email

Company Name

Address

Spam Block (Please leave this blank)

all fields required

Thank you

Your message has been sent. We will be in touch shortly.

Message not sent

Sorry, your message could not be sent at this time. Please try again later, or contact Restek or your local Restek representative via phone.

www.restek.com/Contact-Us