The value of metals testing for risk management and ...

© 2018 Emerald Conference

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The value of metals testing for risk management and product safety

Anthony Smith, Ph.D, Chief Science Officer,

OTCQB: EVIO

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OTCQB: EVIO

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SERVE CONSUMER DEMAND MAINTAIN HIGH STANDARDS ADVISORY SERVICES

EDUCATION

REGULATORY SUPPORT

PROCESS OPTIMIZATION

RESEARCH

FORMULATION

SAFETY

HEALTH

COMPLIANCE AND R&D TESTING

ABOUT EVIO LABS

Provider of accredited analytical testing and industry research in

7 different North American states & provinces

Support Health, Safety, Education

ORELAP Accredited Cannabis Testing Labs

in OR; ISO 17025 in CO, FL, CA, MA &

Alberta, CA

Expertise to Support R&D, Product

Formulation, Grow Optimization


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Heavy Metal Contamination Standards & Limits:

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EU: EC Regulation 1881/2006 Maximum Levels for Contaminants in FoodstuffsAs 0.1-0.3 ppm, Cd 0.1-0.1 ppm, Pb 0.01-0.5 ppm, Hg 0.1-1.0 ppm

UN: Codex Standard 193-1995 General Standard for Contaminants and Toxins in Food and Feed

As 0.1-0.5 ppm, Cd 0.2-0.9 ppm, Pb 0.1-0.3 ppm, Hg 0.1-1.6 ppm

FDA: Has Set Standards for Some Foodstuffs, e.g. Shellfish, Children's Foods, Fruit

Juices and Bottled Water.


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Heavy Metal Contamination:

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Average Inorganic Arsenic, Cadmium and Lead in CarrageenanProduct Average Arsenic Average Cadmium Average Lead Number of Samples

Carrageenan 181 ppb 449 ppb 251 ppb 10

Cadmium and Lead in Infant/Toddler Foods

Product Category Average Cadmium (ppb)

Range of Cadmium (ppb)

Average Lead (ppb)

Range of Lead (ppb) Number of Samples

Cereal - Infant/Toddler (rice) 20.3 8.5 - 43.0 15.6 5.0 - 82.0 76Cereal - Infant/Toddler (multigrain) 47.7 43.0 - 52.0 7.2 6.0 - 8.0 6Cereal - Infant/Toddler (non-rice) 20.4 4.6 - 63.3 4.8 0.4 - 17.0 30

Apples 1.8 1.7 - 3.5 3.3 3.3 10Cereal - Oat Ring 13.1 6.1 - 27.4 7.8 3.3 - 16.4 30

Grapes 2.8 1.7 - 6.4 3.7 3.3 - 7.6 10Juice - Grape 1.3 0.1 - 5.1 5.6 0.3 - 41.3 30

Juice Boxes and Pouches 0.5 0.1 - 1.7 3.3 0.3 - 17.0 40Peanut Butter 71.2 23.5 - 235 5.3 3.3 - 45.2 29

Quinoa 39.2 0.4 - 61.0 22.2 0.4 - 98.0 30Raisins 1.9 1.6 - 5.1 18.1 1.8 - 151 23

Stage 2 Toddler Foods 5.7 1.7 - 31.1 5.2 1.0 - 22.2 35Teething Biscuits 9.2 1.7 - 33.4 12.0 2.0 - 131 27

Toddler Puffs 19.3 4.2 - 29.0 19.1 3.3 - 91.0 31

“Although the FDA has set specific levels for arsenic, lead, cadmium, and mercury in a variety of foods, more generally, the FDAhas—and uses—the authority to take action on a case-by-case basis where a particular food is found through routine or targeted testing to be adulterated” --FDA Statement on Metals in Foods


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FDA Sponsored Research:

Mindak WR, et al. (2008) Lead in women's and children's vitamins. J Agric Food Chem. v. 56

Lead Content in Women's and Children's Supplements

Product Form Lead Concentration (ppm)

Estimated Exposure (µg/day) Population Assessment Group

After Baby Boost 1 Tablet/Capsule 2.4 8.97 Pregnant and lactating womenNutriBiotic Ultimate Matrix Tablet/Capsule 1.2 4.92 Adult women

Apex FIT Multivitamin Women's Tablet/Capsule 1.16 1.91 Adult womenRite Aid Prenatal Tablets Tablet/Capsule 1.13 1.31 Pregnant and lactating women

Esteem Total Woman Tablet/Capsule 0.861 3.61 Adult womenPreferred Plus Women's Daily Tablet/Capsule 0.749 1.31 Adult women

Uno Diario Mujeres Tablet/Capsule 0.65 1.05 Adult womenVegan Prenatal Tablet/Capsule 0.63 1.03 Pregnant and lactating women

Maxi Teen Supreme Tablet/Capsule 0.623 0.942 Older children (7+ years)A to Z Naturals Wow! PreNatal Tablet/Capsule 0.622 5.52 Pregnant and lactating women

Women's One Daily Tablet/Capsule 0.611 1.21 Adult womenWhole Source Complete formula For Women Tablet/Capsule 0.569 1.81 Adult womenGenSpec VF-1 for African American Females Tablet/Capsule 0.562 3.4 Adult women

GNC Women's Ultra Mega Active Tablet/Capsule 0.529 1.87 Adult womenVitamin Source Prenatal Complete Tablet/Capsule 0.528 4.73 Pregnant and lactating womenGNC Women's Prenatal with Iron Tablet/Capsule 0.526 1.63 Pregnant and lactating women

Perry Prenatal Tablet/Capsule 0.52 0.667 Pregnant and lactating womenKal Enhanced Energy Teen Complete Tablet/Capsule 0.513 1.78 Older children (7+ years)

ppm

Num

ber o

f Sam

ples


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Best resource for “typical” heavy metal content in market foods:


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Enough about food and supplements; What about smoked or inhaled products?

Are there manufacturing control limits or regular testing of tobacco and cigarettes?

Reported metals in US cigarettes:

Arsenic 0 - 0.24 ppmCadmium 0.46 - 6.48 ppmChromium 0.06 - 1.11 ppmNickel 0.07 - 1.19 ppmLead 0 - 1.58 ppm

“The average metal concentrations observed per gram of unburned tobacco were comparable to amounts found in cigarettes on the US, Canadian, and Brazilian markets, but less than those found in cigarettes purchased in China”

Caruso RV, et al. (2014) Int J Environ Res Public Health. 11(1)

Ashraf MW (2012) Sci World J. ID 729430Bailey EJ, et al. (1957) Br J Cancer. 11(1)Panta YM, et al. (2008) J Analysis and Applied Pyrolysis. 83(1)

Estimated Daily Exposure

Metal conc.Cigarette wt.Mean transfer rate

X Cigarettes per day

“Median estimated availabilities of As, Cd, and Cr exceed the ‘no significant risk levels’ (NSRL) … as defined by the State of California… all participants’ estimated exposures to Cd would exceed the NSRL, while 50% would exceed the NSRL for As. The estimated potential exposure to Pb is approximately 1/3 of the maximum daily dose (MADL)”

Reported metal content in cigarettes and cigars in AsiaArsenic 20 – 50 ppmCadmium 0.9 – 2.8 ppmLead 1.6 – 3.6 ppmMercury 0.02 – 0.1 ppm


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Are there manufacturing control limits or regular testing of tobacco and cigarettes?

HPHCs in Cigarette Smoke

HPHCs in Smokeless Tobacco

HPHCs in Roll-your-own Tobacco

Acetaldehyde Acetaldehyde Ammonia

Acrolein Arsenic Arsenic

Acrylonitrile Benzo[a]pyrene Cadmium

4-Aminobiphenyl Cadmium Nicotine

1-Aminonaphthalene Crotonaldehyde NNK

2-Aminonaphthalene Formaldehyde NNN

Ammonia Nicotine

Benzene NNK

Benzo[a]pyrene NNN

1,3-Butadiene

Carbon monoxide

Crotonaldehyde

Formaldehyde

Isoprene

Nicotine

NNK

NNN

Toluene

Abbreviated List of Harmful and Potentially Harmful ConstituentsReporting Harmful and Potentially Harmful Constituents in Tobacco Products and Tobacco Smoke Under Section 904(a)(3) of the Federal Food, Drug, and Cosmetic Act

“FDA recognizes that industry may be unable to meet the deadline due to current testing limitations. In recognition of this, the draft guidance identifies 20 HPHCs from the full list of 93 HPHCs, for which testing methods are well established and widely available. FDA is currently exercising enforcement discretion to require reporting about these 20 constituents.”


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0 . 0 0 . 5

C A O t h e r & F L

C A I N H

C A O t h e r & F L

C A I N H

C A O t h e r & F L

C A I N H

C A O t h e r & F L

C A I N H

2 3

M e t a l s A c t i o n L i m i t s F o r D a t a i n T h i s S t u d y

P P M ( µ g × g- 1

)

L e a d

C a d m i u m

A r s e n i c

M e r c u r y

C A L O Q F L L O Q


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Instrument and Method Slide:

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• Shimadzu ICPMS-2030 Systems

• Sample preparation– Microwave digestion in Aqua Regia

• Calibration and QCs

• Blank – Consisting only of the reagents used for digestion and dilution.

• Fortified Blank – Identical to the blank sample, but spiked with 5 ppb As, Cd, Hg, and Pb.

• Matrix – Reagents used for digestion and dilution, along with ~0.5 g cannabis flower

• Fortified Matrix – Identical to the matrix sample, but spiked with 5 ppb As, Cd, Hg, and Pb.

• Validation and method performance (FL and CA)


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Heavy Metals in Florida Cannabis:

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• Over 7100 unique samples tested (October 2017 – February 2019)• Cannabis flower, Concentrates & Extracts and CIPs• ISO 17025, validated method (Shimadzu ICP-MS with microwave digestion)

Study statistics:Analyte LOD (ppm) LOQ (ppm) Action Limit (ppm) # above LOD # above LOQ % above LOQ # Fails Fail %Mercury 0.001 0.2 3 956 23 0.3% 2 0.0%

Lead 0.001 0.2 0.5 1456 159 2.2% 69 1.0%Cadmium 0.001 0.2 0.5 901 124 1.7% 37 0.5%Arsenic 0.001 0.2 1.5 1152 205 2.9% 56 0.8%


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Figure 1: Heavy Metals Detected Above LOQ (0.2 ppm) in Cannabis Flower vs Concentrate & Extract Samples

0 1 2 3 4 5 6 7 8 9 1 0

M e r c u r y ( C & E )

M e r c u r y ( F l o r )

L e a d ( C & E )

L e a d ( F l o r )

C a d m i u m ( C & E )

C a d m i u m ( F l o r )

A r s e n i c ( C & E )

A r s e n i c ( F l o r )

4 0 6 0 8 0 1 0 0

M e t a l s A b o v e L O Q ( 0 . 2 P P M ) i n F l o w e r a n d C o n c e n t r a t e &

E x t r a c t S a m p l e s

P P M ( µ g × g- 1

)

A b o v e C a l .


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Data Trend Analysistypical Failed sample has more than one target detected above LOQ

Value to CustomersValidating components, ingredients, processesStory slides

1. Tracking down Cadmium in two producers operations2. Lead contamination from process hardware


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production_method type Analyte Result (PPM)Butter/Animal Fat Concentrate Lead 80.1Butter/Animal Fat Concentrate Lead 68Butter/Animal Fat Concentrate Lead 61.1Butter/Animal Fat Concentrate Lead 21.8Butter/Animal Fat Concentrate Lead 18.1Butter/Animal Fat Concentrate Lead 10.8Butter/Animal Fat Concentrate Lead 9.78Butter/Animal Fat Concentrate Lead 6.68Butter/Animal Fat Concentrate Arsenic 4.98Butter/Animal Fat Concentrate Lead 1.82Butter/Animal Fat Concentrate Arsenic 1.51Butter/Animal Fat Concentrate Arsenic 1.43CO2 Crystalline Solid Arsenic 11CO2 Extract Arsenic 6.9CO2 Distillate Arsenic 4.7CO2 Extract Arsenic 4.69CO2 Distillate Mercury 4.51CO2 Extract Arsenic 4.06CO2 Crystalline Solid Lead 3.93CO2 Distillate Lead 3.813CO2 Distillate Arsenic 3.3CO2 Extract Arsenic 3.22CO2 Distillate Arsenic 3.19CO2 Distillate Arsenic 3.13CO2 Extract Arsenic 2.95CO2 Distillate Arsenic 2.86CO2 Distillate Arsenic 2.69CO2 Extract Arsenic 2.67CO2 Extract Arsenic 2.43CO2 Distillate Mercury 2.38CO2 Distillate Arsenic 2.3CO2 Distillate Arsenic 2.3CO2 Distillate Arsenic 2.22CO2 Distillate Arsenic 2.11CO2 Distillate Cadmium 2.09CO2 Extract Arsenic 1.99CO2 Extract Arsenic 1.99CO2 Extract Arsenic 1.79CO2 Extract Arsenic 1.78CO2 Extract Arsenic 1.67CO2 Extract Arsenic 1.65


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Isolating ‘industrial contamination’ in clients ag processes

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• Prelimiary routine sampling and testing of early flower development showed intermittent ‘streaks’ of Cd in their greenhouses

• Data table

Type Target PPMFlower-Cured Cadmium 0.247Flower-Cured Cadmium 0.339Flower-Cured Cadmium NDFlower-Cured Cadmium 0.234Flower-Cured Cadmium 0.499Flower-Cured Arsenic 0.308Flower-Cured Cadmium 0.225Flower-Cured Cadmium 0.266Flower-Cured Arsenic 0.286Flower-Cured Cadmium NDFlower-Cured Cadmium NDFlower-Cured Cadmium 0.495Flower-Cured Cadmium 1.39Flower-Cured Cadmium NDFlower-Cured Cadmium 1.07


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Isolating ‘industrial contamination’ in clients ag processes

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• Prelimiary routine sampling and testing of early flower development showed intermittent ‘streaks’ of Cd in their greenhouses

• Data table

Type Target PPMFlower-Cured Cadmium 0.247Flower-Cured Cadmium 0.339Flower-Cured Cadmium NDFlower-Cured Cadmium 0.234Flower-Cured Cadmium 0.499Flower-Cured Arsenic 0.308Flower-Cured Cadmium 0.225Flower-Cured Cadmium 0.266Flower-Cured Arsenic 0.286Flower-Cured Cadmium NDFlower-Cured Cadmium NDFlower-Cured Cadmium 0.495Flower-Cured Cadmium 1.39Flower-Cured Cadmium NDFlower-Cured Cadmium 1.07

aerial parts Cadmium ND - 0.5 ppmrockwool bits Cadmium 5.3 - 80.2 ppmroot tissue Cadmium 0.02 – 0.08 ppmsoil Cadmium NDother p.o.e, e.g. water, foliar spray,. etc. ND


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Screening vape cartridges and filling equipment

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• Sample prep scheme (1 cart, opened and rinsed with aqueous 20% Nitric Acid)• Range of dilutions used for scale• QC’s: Blank leachate and leachate solution spiked w/ standards

Sample Pb (ng/mL) Descr.Blank leachate ND QCLCS leachate 9.2 QC

046A 176.0 V1

046B 2940.0 V1

046C 465.0 V1046D 560.0 V1046E 1360.0 V1

046 mean 1100.2047A 270.0 Z Cell

047B 184.0 Z Cell

047C 395.0 Z Cell

047D 211.0 Z Cell

047E 253.0 Z Cell

047 mean 262.6LCS recovery 92.3%


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Scientific Conclusions:

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Technical…

• The main technical barrier is risk for sample-to-sample carryover and maintaining clean blanks

• In California, acid+microwave digestion of ½ gram samples may incur increased safety risk

Practical…

• The gathering of large heavy-metals data sets for a particular commercial commodity is unprecedented and has epidemiological implications

• It is easy to contaminate a cannabis product without having heavy metals in your soil• Risk management, process control and surveillance can keep heavy metals out of your product


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