CEO Response to Failed GC/MS Reports

January 29, 2018 - Update to GC-MS Results on Carterii, Myrrh, & Birch

 

As promised, I am providing an update on our 6 step action plan previously outlined on January 5th. Our Myrrh and Frankincense Carterii batches were re-tested by Phytochemia (http://www.phytochemia.com/en/home/). We are still waiting on results from the Birch. Phytochemia disagrees with Dr. Robert Pappas that the Carterii was significantly adulterated, but agrees that the Myrrh was significantly adulterated with castor oil. I was hoping to release information to the public a little sooner than today, but we have been waiting to see if Dr. Robert Pappas and Phytochemia could come to a consensus, but as of now, that doesn't seem to be the case. Rather than providing you with our assessment of the correspondence, we believe that the EO community has the right to review the information and draw their own conclusions. Dr. Robert Pappas states that our batches of Frankincense Carterii were 'significantly' adulterated with Castor oil, but Phytochemia disagrees that 1% is significant or represents malicious intent. We also have an official statement of defense from the distiller that there was never any wrongdoing and that the .1% peak of ricinelaidic acid is a naturally occurring fatty acid from the resin that was distilled. The distiller also defends any wrong doing with the Myrrh.

 

 

STATEMENT FROM PHYTOCHEMIA - (click here to see their GC-MS for Carterii & for Myrrh)

 

"The preliminary testing we have done using a modified protocol with an internal standard allows me to estimate the content of castor oil at about 1% of the sample. At such level, I would not suggest that this is adulteration, rather unwanted contamination, for example by contact with a contained having been in contact with castor oil previously.

 
For the sake of transparency, here is the method applied: we spiked an aliquot of your frankincense oil with a solution of known concentration of tridecanoic acid, then treated the mixture for FAMEs analysis. We used 50 µL of oil (before spiking) whereas we typically use 3 µL for derivatization, hence reaching a much higher sensitivity. Under these conditions, we were able to readily detect the methyl ricinoleate peak (indicative of castor oil). Calculating based on the methyl tridecanoate peak, we were able to estimate the content of ricinoleic acid at a bit less than 7 mg/mL of oil. We neglected the contribution of glycerol in the process, as this induces a minor deviation only - we plan on refining the technique in the future, but now we mostly wanted to give you an answer quickly. Typical castor oil contains 80+% of ricinoleic acid, which makes a maximum estimated total content of fatty acids of 8.6 mg/mL, or 0.86%. If however the oil involved is similar to the one observed in your myrrh sample, which had only 66% castor oil (which had us say that the carrier was not only castor oil, but also something else), the content would rather be 10.5 mg/mL, or 1.05%.
 
Anyhow, this makes a value quite close to 1%. There is little economical argument that would justify adding such a small amount of carrier to extend an oil for an outright adulteration, thus this is why we rather suspect unwanted contamination somewhere in the process.
 
We will now work toward streamlining this technique so that all your samples will be checked systematically under the pilot project. We will probably also refine the calculation method."

 

 


DR. ROBERT PAPPAS RESPONSE TO 
PHYTOCHEMIA RESULTS

 

"Sure, I agree there is less castor in the Frankincense than the myrrh, could be like 5% or less.  The FAME testing can’t always catch it, which is why you have to know what marker to look for and that’s not really info that we want to share for obvious reasons.  Hard to say what could have happened, perhaps the oil I got was not the same oil. Maybe some contamination? Who knows. The distiller was likely not to blame."

 

 

 

STATEMENT FROM DISTILLER

 

"We were extremely shocked to hear about a concern with our essential oil of olibanum in which a substantial amount of castor oil was found. We vehemently deny any wrongdoing and any kind of adulteration with castor oil in our product. In the last two years, we have imported over 150 tons of olibanum gums carterii. On these gums we produce both the essential oil (with a yield around 7%) and the resinoid (direct ethanol extraction). Needless to say that this product is one of the most important and strategic in our line. Therefore, we cannot accept these accusations and need to find a way to clear our reputation.

In the past, we have imported some goods that had been adulterated with castor oil.  (sandalwood , patchouly and ylang ylang.)  Castor Oil is a very difficult product to determine and especially to quantify. There are however several methods to find out if such an adulteration is present, especially  in substantial amount .

The blotting paper method : this is how the old generations, pre GLC – GCMS, were checking those kind of adulteration. You put one drop of the suspicious essential oil on a piece of blotting paper. The stain will spread abnormally if castor oil is present. On Lot 170004420, we see no such things. We ask you to make this simple test if possible.

The residues content : a more straightforward method. It is possible to redistill under vaccum the essential oil of olibanum. The distillating point of castor oil is very high, therefore it will not be distilled with the rest of the essential oil. By weighting the residues that are not redistilled, it is possible to see if the product contains a heavy oil. Typically, an essential oil of olibanum that is very terpenic, will have around 6% to 7% of residues.  If the amount of residues is higher that could mean that the product has been adulterated. The lot 170004420, shows a residue content of 6%. 

The density : the density of castor oil can be from 0.960 to 0.969 as per the information given to us by Brenntag, largest importer of castor oil (from India) in Europe (attache dis a TDS from Brenntag). As per our certificate of analysis (attached), the lot 170004420 has a density of 0.8629 (for a range that can go from 0.850 to 0.892). Just for the sake of argument, it is easy to understand that a  substantial amount  of castor oil  will put the density outside of the specs of a pure essential oil.

GLC thin layer analysis : a more sophisticated method that needs a special equipment (which we do not have internally). This is a comparison method between a thin layer analysis of the lot that is suspicious with the thin layer analysis of castor oil. By comparison, it can be seen if the product has been adulterated with castor oil and with how much quantities. There is a lab in France called Phytocontrol that can do that.

Normal GLC comparisons : castor oil is really a column killer but regular GLC analysis can show an adulteration. An essential oil GLC will be defined by two main variables : the retention time and the integrated value of the peaks both in Area and Height. Castor oil will not affect the retention times but will affect the integrated values. The GLC will only integrate the peaks that it can see. Meaning that if  a substantial amount  of castor oil is present in the oil then the integrated peaks will be downsized both in Area and Height. I gave you an example attached : we have analysed a batch of essential oil of olibanum and a batch of the same batch adulterated 50% with castor oil. Please see the results. That means that if you have a lot of olibanum that you know is not adulterated (from another company obviously) and that you check the integrated values and compare it with our  substantially adulterated  batch, the total  integrated values should be MUCH lower in our batch. This is for us the ultimate proof.

I have to admit that there might be other ways of checking the castor oil content in an essential oil but these are the only ones I am familiar with. Our lot 170004420 passed 1,2,3 and 5. We have not tested 4. This is already for us a good proof that our product is not adulterated.

In your email, you mention the presence of a marker in the essential oil, that shows the presence of castor oil. This marker is the ricinelaidic acid contained 0.1% (that value has no meaning as this is a qualitative gcms analysis and not a GLC analysis but still it is very low). I noticed that this peak is surrounded by frankincence unidentified peaks. Probably peaks coming from the acid contained in the gums of olibanum. When gums are distilled under high vaccuum, you always get some traces of gums in the essential oil. Could it be that the identified ricilinoeic acid is not riciloneic acid but rather another unidentified frankinsense peak ? I am getting rather pointy but this peak is not a marker but rather for you an external peak that you are searching in the essential oil. There are two markers in the essential oil of olibanum that are cembrenol and encensol, two peaks that are absent from your analysis.

This is to add to the file but you can see that a quantitative analysis and a qualitative analysis give some slightly different results even if comparable.

The laboratory PhyrtoChemia claims that castor oil contains many fatty acids, 80% of which are riciloenic acid. It is my understanding that the amount of 0.1% found in our batch of essential oil (even if maybe there could be a slight difference) would indicate a very small amount of castor oil in this product (around 0.125%). If this is the case, which we again deny, one could argue about a pollution but definitely not an adulteration.

We are in a weird spot as we have to demonstrate that we are not thieves. We do not pretend to know everything about essential oils. They are natural complex substances. In fact we would be more than happy to invite you in Italy while we are distilling the gums of olibanum, myrrh, elemi, galbanum or opoponax to show you the distillation process."

 

PHYTOCHEMIA'S RESPONSE TO DISTILLER'S COMMENTS

 

Distiller: We were extremely shocked to hear about a concern with our essential oil of olibanum in which a substantial amount of castor oil was found.

PhytochemiaTo me, 1% is not substantial - I will remind here that we honestly had not seen any problem at once with the oil, and were prompted to look further because of the claims of another analyst.

 

DistillerWe vehemently deny any wrongdoing and any kind of adulteration with castor oil in our product.

Phytochemia I still do not think that this is intentional either.

 

Distiller: In the last two years, we have imported over 150 tons of olibanum gums carterii. On these gums we produce both the essential oil (with a yield around 7%) and the resinoid (direct ethanol extraction). Needless to say that this product is one of the most important and strategic in our line. Therefore, we cannot accept these accusations and need to find a way to clear our reputation.  In the past, we have imported some goods that had been adulterated with castor oil.  (sandalwood , patchouly and ylang ylang.)  Castor Oil is a very difficult product to determine and especially to quantify. There are however several methods to find out if such an adulteration is present, especially  in substantial amount .  The blotting paper method : this is how the old generations, pre GLC – GCMS, were checking those kind of adulteration. You put one drop of the suspicious essential oil on a piece of blotting paper. The stain will spread abnormally if castor oil is present. On Lot 170004420, we see no such things. We ask you to make this simple test if possible.

PhytochemiaWe have not done that testing precisely (but my instinct would tell me 1% is not enough to significantly change the diffusivity of the sample), however we have made a spot dry-out test - simply, you had asked for more robust testing in the past, so we do not report those results to you. We still use them as quick checks on some occasions. A drop of the sample on a sheet of paper did leave a very faint stain after 1 h in the oven at 100 celsius, but not clear enough to jump to conclusions.

 

DistillerThe residues content : a more straightforward method. It is possible to redistill under vaccum the essential oil of olibanum. The distillating point of castor oil is very high, therefore it will not be distilled with the rest of the essential oil. By weighting the residues that are not redistilled, it is possible to see if the product contains a heavy oil. Typically, an essential oil of olibanum that is very terpenic, will have around 6% to 7% of residues.  If the amount of residues is higher that could mean that the product has been adulterated. The lot 170004420, shows a residue content of 6%.

PhytochemiaThe problem here lies with potential natural variability, combined with the very low amount of castor oil involved. If indeed the content is about 1%, or even less, the residue may still fall within regular expectations, and go unnoticed.

 

DistillerThe density : the density of castor oil can be from 0.960 to 0.969 as per the information given to us by Brenntag, largest importer of castor oil (from India) in Europe (attache dis a TDS from Brenntag). As per our certificate of analysis (attached), the lot 170004420 has a density of 0.8629 (for a range that can go from 0.850 to 0.892). Just for the sake of argument, it is easy to understand that a  substantial amount  of castor oil  will put the density outside of the specs of a pure essential oil.

PhytochemiaSupposing perfect additivity of volumes, 1% of castor oil of density 0.965 with 99% of an oil with density of say 0.8700 will give a density of 0.8710. This can thus go easily unnoticed.

 

DistillerGLC thin layer analysis : a more sophisticated method that needs a special equipment (which we do not have internally). This is a comparison method between a thin layer analysis of the lot that is suspicious with the thin layer analysis of castor oil. By comparison, it can be seen if the product has been adulterated with castor oil and with how much quantities. There is a lab in France called Phytocontrol that can do that.

PhytochemiaWe could probably make a thin layer chromatography of the sample too, but in the end, the FAMEs testing is more specific.

 

DistillerNormal GLC comparisons : castor oil is really a column killer but regular GLC analysis can show an adulteration. An essential oil GLC will be defined by two main variables : the retention time and the integrated value of the peaks both in Area and Height. Castor oil will not affect the retention times but will affect the integrated values. The GLC will only integrate the peaks that it can see. Meaning that if  a substantial amount  of castor oil is present in the oil then the integrated peaks will be downsized both in Area and Height.

PhytochemiaThis is what made us miss the castor oil altogether in the first place. Back with your other sample that had about 40% castor oil, the total peak area dropped accordingly, just as your supplier mentions (I must mention at this point, all the methodologies he is talking about are valid, and show that he knows his trade). But under 5% of dilution, the variation in total peak area can fall within the expected inter-injection variation that one can find only by injecting repetitively the same sample on the same instrument. 1% is definitely something we cannot detect with this method alone, hence why we had reported nothing in the first place. 

 

DistillerI gave you an example attached : we have analysed a batch of essential oil of olibanum and a batch of the same batch adulterated 50% with castor oil. Please see the results. That means that if you have a lot of olibanum that you know is not adulterated (from another company obviously) and that you check the integrated values and compare it with our  substantially adulterated  batch,

PhytochemiaThis is the key here: for the frankincense, the lot is not substantially adulterated

 

Distiller:  the total integrated values should be MUCH lower in our batch. This is for us the ultimate proof.  I have to admit that there might be other ways of checking the castor oil content in an essential oil but these are the only ones I am familiar with.

PhytochemiaThe two others checks we have on file for this whole situation are the "marker" suggested by Robert Pappas, and the FAMEs testing we performed. The FAMEs methodology consists in digesting the sample in acid (this releases the fatty acids from glycerides, the form under which they are found within a vegetable oil), then turning them into their methyl esters to make them easier to analyze, hence the name: Fatty Acids Methyl Esters. The methyl esters can then be analyzed by GC methods, and compared to other samples and literature. The ricinoleic acid methyl ester was found in the frankincense sample with our modified methodology that compensates for the low amount of castor oil present, and validated both by GC-MS and identity of retention time with the same molecule found from a castor oil sample

 

Distiller: Our lot 170004420 passed 1,2,3 and 5. We have not tested 4. This is already for us a good proof that our product is not adulterated.  In your email, you mention the presence of a marker in the essential oil, that shows the presence of castor oil. This marker is the ricinelaidic acid contained 0.1% (that value has no meaning as this is a qualitative gcms analysis and not a GLC analysis but still it is very low.

PhytochemiaI have to disagree here, but with much caution. As much as I am unsure that the marker is indeed a marker, the very notion of marker pretty much eliminates the relevance of amount. For example, any quantity of dihydrolinalool found in a linalool-rich oil will indicate addition of synthetic linalool. The marker in itself is typically a minor constituent, with very small concentrations, and is not expected to be present in large amounts even if the dilution is of a large amount. This is a semantic precision, however, and does not change the numbers at hand here

 

DistillerI noticed that this peak is surrounded by frankincence unidentified peaks. Probably peaks coming from the acid contained in the gums of olibanum. When gums are distilled under high vaccuum, you always get some traces of gums in the essential oil. Could it be that the identified ricilinoeic acid is not riciloneic acid but rather another unidentified frankinsense peak

PhytochemiaThe peak pointed out by Robert Pappas features a very, very specific mass spectral signature, and can hardly be confused with anything else that would come from the frankincense (typically diterpenic compounds, which exhibit a very different behavior in mass spectrometry)

 

DistillerI am getting rather pointy but this peak is not a marker but rather for you an external peak that you are searching in the essential oil

PhytochemiaIt also is a matter of semantics - there are markers for essential oils, and markers for other things (such as synthetic carvone, linalool, etc.) A marker just confirms the fact that a given ingredient is present.

 

DistillerThere are two markers in the essential oil of olibanum that are cembrenol and encensol, two peaks that are absent from your analysis.

PhytochemiaBy the way, we reported both incensole and serratol in our report, both of which are markers for frankincenses. The debate here is not whether or not this is initially frankincense oil, which is certainly the case, but rather if it is pure.

 

Distiller: This is to add to the file but you can see that a quantitative analysis and a qualitative analysis give some slightly different results even if comparable.  The laboratory PhyrtoChemia claims that castor oil contains many fatty acids, 80% of which are riciloenic acid. It is my understanding that the amount of 0.1% found in our batch of essential oil (even if maybe there could be a slight difference) would indicate a very small amount of castor oil in this product (around 0.125%) 

PhytochemiaThere is a confusion of several concepts here. The fatty acids which we have monitored are, originally, contained as glycerides within the sample, and will not show whatsoever during the GC analysis. The ricinelaidic acid lactone that Robert Pappas reports is something else: presumably, a small compound that is claimed to be present in the crude castor oil (without any chemical modification), and that can be seen during a GC run without any modification (by the way, we have not detected it during the classical GC run). One cannot apply the 80% of ricinoleic acid we took as a basis for our hypothesis of content and infer that to the 0.1% of ricinelaidic acid lactone reported by Mr. Pappas, since the ricinoleic acid we are monitoring comes essentially from the cleaved glycerides, and not from the conversion of the very small amounts of ricinelaidic acid lactone.

 

DistillerIf this is the case, which we again deny, one could argue about a pollution but definitely not an adulteration. 

PhytochemiaThis is quite much what we suspect at this point.

 

 

 

As new dialogue or findings are made available, we will update this page.

 

Now, in regards to our action plan, I am very pleased to provide the community with the internal progress we have made.  First, let me say that we will still be honoring the promises we made regarding any customers that have purchased Myrrh, Carterii, or Birch from us in the last 12 months.  You can read the statements from January 5th to see what options are available to you.  These 3 oils are still temporarily removed for sale from our website, but we have received new lots of Myrrh and Carterii at our shipping facility in Utah.  Once we have posted the new GC-MS reports to the website, we will open up these oils for sale again on the website.

 

We have been testing a new machine that prints the batch numbers on our bottles.  This is part of our commitment to move towards full USDA certification.  Please understand, this certification does not change the quality of the oil we have been selling as we have always fully committed to selling the highest quality organic essential oils from the very beginning.  The certification simply provides 3rd party verification of our internal processes and paper management.

 

Moving forward, we are now GC-MS testing every batch of oil before we begin bottling.  When our overseas batches land in California, we are sending a sample for 3rd party testing to Phytochemia in Canada.  Also, we have purchased state-of-the-art machinery for our own internal testing.  Any time we break down our batches to ship to our facility in Utah, Dr. Hussam will be re-testing the batch to confirm the purity.  I was in California last week inspecting our lab being set up for our "last mile" testing.  Here are a few pictures of me with Dr. Hussam and close-ups of our new equipment. 

 

 

 

GCMS2GCMS3GCMS4

 

 

 

In closing on this update, I would just like to say how grateful I personally am to our customers.  I was extremely touched to see members of our JB family rally around us.  The amount of love and support we have received was unprecedented and we certainly felt it when one of our affiliates drove from Colorado to show us a crowdsourced video collage of our customers sharing their love.  Here is a link to the video that she posted on Facebook https://www.facebook.com/ChisholmJenn/videos/10155159029541899/

 

We are fully committed to continuing to provide the highest quality 100% pure essential oils in the world at the lowest possible prices and the events this month has made us better, stronger, and more prepared to serve you.

 

With Love,

Adam Wilkinson

CEO

Jade Bloom

 

 

 

 

January 5, 2018

 

My name is Adam Wilkinson; I’m the CEO of Jade Bloom.  Yesterday, it was brought to our attention that some of our oils did not pass GC/MS testing performed by Dr. Robert Pappas.  I spoke with Dr. Robert Pappas on the phone this morning regarding the tests, and I can confirm that the tests he performed were on bottles of Jade Bloom’s Sweet Birch, Frankincense Carterii, and Myrrh.  We have sent follow-up samples directly to Dr. Pappas from the same batches of oil to confirm the adulteration.  

 

I appreciate the opportunity to personally address this issue, as the quality of our oil is the one single effort that takes priority over all else.  We want the essential oil industry to know 2 things: 1) if the secondary analysis from Dr. Robert Pappas reveals the same results, there was never any deliberate or malicious intent by Jade Bloom to mislead our loyal customers and 2) we take full responsibility and we will provide adequate restitution for any oil that ever leaves our bottling center that is anything, but 100% pure.

 

I appreciate Dr. Robert Pappas follow up response to the EOA thread regarding his tests.

 

Robert Pappas - Hi would just like to let people know that these three cases of Jade Bloom are not easy adulterations to detect and would get past most labs because just a surface GCMS run by someone who isn't extremely experienced with the less obvious adulterations in the EO world would completely miss these and think that the oils were authentic. The detection of adulteration in these case all rely on trace marker peaks which will get past most labs. So before you cast too harsh of a judgement I would just tell you that there is not a single EO company out there ANYWHERE that has not sold an adulterated oil at one time or another. I know there are those of you out there that think that your favorite companies are perfect and their oils are always as pure as the driven snow 100% of the time, but that is just not the case. After doing this kind of analytical work for over 22 years for hundreds of different companies I promise you that NOBODY is above selling an adulterated oil. Some companies of course spend more resources than others to avoid this, but none have completely eliminated the possibility. The most important thing to watch is how the company handles the bad news. So far the CEO of Jade Bloom has reached out to me and I think he is making a good faith effort to get to the bottom of it and rectify the situation. Only time will tell but so far I get the feeling that this company wants to do the right thing.”

 

On the phone, it was encouraging to hear Dr. Pappas say that if our entire batch was adulterated in the same way, it still isn’t unsafe for customers to use.  We are constantly warning people about how some adulterated oils can be dangerous if they have harmful chemicals in them.  We also actively educate consumers that they should be demanding a copy of the GC/MS report for whichever oils they choose to buy.  Now, here we find ourselves potentially standing in the same shoes of many of those companies that have either internally or unintentionally adulterated their oils and people are waiting to see how we respond.  I believe Dr. Pappas has a mature insight on our industry when he says “NOBODY is above selling an adulterated oil” and “I get the feeling that this company wants to do the right thing.”  We absolutely will do the right thing and here is the action plan we have put in place so far:

 

ACTION PLAN

  1. Sweet Birch, Frankincense Carterii, and Myrrh have been temporarily removed for sale from our website pending a secondary analysis to be performed Dr. Robert Pappas.
  2. Our drums of these oils have been isolated until our investigation is complete and any proprietary blends containing these oils have also been deactivated.
  3. We are offering a full refund to any customer that have purchased Sweet Birch, Frankincense Carterii, or Myrrh in the past 12 months.  We will be paying double the money back to customers that choose a refund in loyalty points instead of cash.  There should be zero incentive for companies that sell adulterated oil to take profits and leave the consumers with something they didn’t agree to purchase.  Contrarily, we want our customers to know as Jade Bloom grows, if we EVER sell an oil that gets past our quality control as anything less than 100% pure, our policy on how we handle it will hurt us.  Our policy of paying customers double can only provide incentive for ensuring every oil is 100% pure.  Please contact our customer support team and let us take care of you. 
  4. We are in the process of moving towards USDA organic certification for our oils and we will have it this year.
  5. Starting in February, newly bottled oils will include a stamp on the bottle to easily identify the batch from which the oil was derived.
  6. We have hired P.h.D. Chemist Dr. Hussam to perform GC/MS tests on all batches going the last mile to Utah.  Our GC/MS machine should be fully operational by next week and we expect to produce 2 GC/MS reports for every batch of oil.  We source our oils from all over the world with our main distillery in India.  Stephanie and I will be visiting our distillery and some farms in India next month for quality control, but that operation only distills about 60% of the oils we sell.  We do require our partner distillers in other parts of the world to GC/MS test our batches before shipping, but we are learning from this potential failure that what arrives in a drum or a tote might not actually match our GC/MS report.

 

Jade Bloom oils have been rigorously tested over the years by 3rd party groups just like EOA.  After shipping a million bottles in 3 years, this is the first report we have seen of our oils not passing test results.  While it’s hard for us to believe how that could be possible, we are learning how it could be possible and we’re moving forward as if the information from Dr. Robert Pappas is representative of our most recent batches of Birch, Carterii, and Myrrh. 

 

By the way, this is not the first time that we have failed.  We took the time to document our list of failures over the past 3 years if you are interested in reading them here: https://jadebloom.com/failure.html

 

Jade bloom exists to change the way people think about health and our mission is to provide the highest quality 100% pure essential oils at the lowest price points possible.  If we allowed price to take precedence over quality with these 3 oils then please accept my personal apology along with my personal reassurance that we WILL do better.  With 6 kids, I understand how important trust is, but also how fragile it can be.  Trust can be so easily broken and the most important asset that will move Jade Bloom one step closer each day to accomplishing our main goal, is the trust of our loyal customer base.  If we have broken that trust with you, please be patient with us as we work to earn it back with you.  I don’t think you will be disappointed in our efforts, but if so please reach out to me personally at [email protected].