Scientific Publication: Analysis of Electronic Cigarette’s Cartridges (Trehy et al. 2011)

[Uncle Willie]

@Vocalek .. I always enjoy your posts and you are a very well spoken young woman ..

I believe we are in the Wild Wild West phase of this industry and I call this the Golden Age of the PV .. there is no way, especially with the growth of the product, that regulation / etc, will not step in, sooner than later ..

I applaud you for fighting the good fight .. but I am afraid that a product based on nicotine will, as you say, "they are going to be regulating the product you know and love so tightly" ..

I don't like it any more than anyone else .. however, it appears to be the only path towards any degree of consistency in this industry ..

I don't fret (much) over the quality and ingredients of the liquid I use .. but I do know that I really don't know what a maker puts in it .. and anything that is ingested, in any form, should have at least a certain degree of expected quality ..

Yes, I know we have regular food scares / and nothing is fully safe .. the arguments been beat to death on the forum ..

 

[kristin]

The objective of this study was to determine nicotine and the nicotine related impurities

All of the resources available to them and this is what they test for?? Wouldn't it stand to reason that a product which contains nicotine would have nicotine-related impurities? And even if these would not be found in the 98% pure nicotine they used as a control, they would be found in the smoke that the user would otherwise be exposed to. And what are the health risks of these impurities? The same would probably be found in low-risk smokeless tobacco, which we know is 99% safer than smoking.

The electronic cigarette was observed to stay lit for approximately 2 sec after the 100 mL puff of air was initially actuated, and the air flow into the washing bottle stopped approximately 4 sec after the 100 mL
puff of air was initiated.

A 2 second puff? That's about 1/3 of a typical puff for most users.

CONCLUSIONS
The gradient elution method was developed to allow for separation of
the nicotine related impurities and for their determination in cartridge
extracts of the electronic cigarettes. Nicotine was shown to be delivered
using electronic cigarette devices although the amount of nicotine delivered will be greatly impacted by the ‘‘smoking’’ habits of the consumer.
Significant labeling issues were found to exist with products in the market
place with respect to product labeling accuracy. Some products were found
to contain high concentrations of nicotine when labeled not to contain
nicotine.

Yippee! They told us that CIXI is a crappy company and the industry needs standards and regulation for proper labeling. Wait...we knew that already. But are there any dangers in the actual vapor?? I guess they can keep saying "We don't know."

The marketing of electronic cigarettes as a healthier alternative to smoking traditional cigarettes has raised some concerns

Is this the kind of government action designed to help us "achieve a meaningful, legal, safe and consistent activity?" How does testing using fresh air and 98% pure nicotine as controls determine if the product really is a healthier alternative to smoking? Shouldn't they be using their considerable resources and comparing them to smoking? The only people this study helps are never-tobacco users who want to use e-cigarettes. This study is designed purely to argue that e-cigarettes aren't 100% safe, not to prove that they are/aren't a healthier alternative to smoking. The users of this product are already smokers who are already exposed to many toxic chemicals beyond nicotine impurities. To ignore that fact is ridiculous and pointless. The only reason to point out such a low risk in e-cigarettes is to discredit them and get them banned. There is simply no other purpose to this when they could be testing for REAL dangers.

While we need the studies showing REAL risks, THIS study is not the kind of government action we need.

I don't oppose testing. I oppose otherwise POINTLESS testing that is designed to imply e-cigarettes are more of a health risk than they actually are.

 

[Vocalek]

Let's turn our attention back to the report. To refresh our memories, this is the abstract for the article.

The objective of this study was to determine nicotine and the nicotine related impurities, that is, cotinine, myosmine, anatabine, anabasine, and b-nicotyrine, in electronic cigarette cartridges, the liquid used to fill the cartridges, and from smoke generated using the electronic cigarette devices. An HPLC method was validated for the determination. Samples of nicotine containing products were purchased via the internet from NJOY, Smoking Everywhere, CIXI, and Johnson Creek. Electronic cigarette devices were purchased from NJOY, Smoking Everywhere, and CIXI. The results from the testing found that (1) the nicotine content labeling was not accurate with some manufacturers, (2) nicotine is present in the ‘‘smoke’’ from electronic cigarettes, and (3) nicotine related impurities contents in cartridges and refills were found to vary by electronic cigarette manufacturer.

Given that objective, you would expect to see some tables in the report that shows the quantities detected of each of the nicotine related impurities for each of the four brands tested, no?

Under the section heading Nicotine Related Impurities in Cartridge Extracts, we find Table 2, which lists the "Nicotine Label Content versus Nicotine Content Found for Cartridges from Three Different Manufacturers."

Smoking Everywhere
0 mg. cartridges - ranged from 0.0 to 0.1 mg.
6 mg. cartridges - ranged from 1.0 to 2.7 mg.
11 mg. cartridges - ranged from 2.7 to 5.2 mg.
16 mg. cartridges - ranged from 4.2 to 6.0 mg.

NJOY
6 mg. cartridge - 5.2 mg.
12 mg. cartridges - ranged from 4.3 to 5.3 mg.
18 mg. cartridge - 6.8 mg.

CIXI
0 mg. cartridges - ranged from 0.07 to 21.8 mg.
16 mg. cartridges - ranged from 0.00 to 21.00 mg.
24 mg. cartridges - ranged from 0.09 to 20.6 mg.

My observations: Either the FDA's extraction methods were a bit off, or all three companies have quality control issues, with CIXI being the absolute worst. But I do find it strange that FDA did not use a consistent number of samples such as 4 cartridges for each label value for each of the companies.

Next up, TABLE 3 "Results from CIXI for Nicotine and Nicotine Related Impurities in Cartridges Expressed as mg=Cartridge"

The column headings were Cotinine, Myosmine, Anatabine, Anabasine, Nicotine, b-Nicotyrine

The report states, "All nicotine containing products contained nicotine related substances. Results shown are representative of impurity levels observed for other manufacturers except for anatabine levels."

Now the curious thing is that none of the other manufacturers offer 24 mg E-......, 0 mg E-......, 0 mg E-rimonabant, 24 mg E-rimonabant, 16 mg E-rimonabant, or 16 mg E-....... Maybe these are popular options in China, but (correct me if I'm wrong) I don't see American men getting all excited about these "flavors". Nevertheless, the FDA lab did find some Myosamine and Anatabine in these flavors, as well as in a product labeled 24 mg, Marlboro Taste. No impurities were found in in the 0, 16, and 24 mg "regular" flavors.

Given all this, how is the reader expected to extrapolate impurity values for the other brands? My guess would have to be that they would have had to list "ND" (for not detected) or "<LOQ" (below the limit of quantification) for all the other samples, and the table would have been unwieldy.

Next we come to the heading Nicotine and Nicotine Related Impurities in Puff Trapping Solutions. This must be the "smoke" referred to in the abstract. The report states, "Although, nicotine related impurities were not detected in the puffs above the LOQ for the electronic cigarettes, this is attributable to the lower nicotine delivery observed and not the absence of nicotine impurities in the smoke."

Translation: Just because there wern't any impurities in the unvaporized liquid, and we couldn't find any in the vapor itself, doesn't mean that those impurities aren't there!!!

In Table 6, again CIXI is the lone e-cigarette vendor displayed, and the values were all ND or <LOQ for the impurities. Nicotine ranged from 50 to 254. Results were expressed in micrograms per thirty 100mL puffs. Table 6 also listed values for a traditional cigarette: 313 Cotinine, 220 Myosmine, 117Anatabine, 540 Anabasine, 4,558 Nicotine, and <LOQ b-Nicotyrine.

I had no argument with their conclusion that the products do deliver nicotine, "although the amount of nicotine delivered will be greatly impacted by the ‘‘smoking’’ habits of the consumer." I also agree that they found significant labeling issues, in view of the wide range of nicotine content in the cartridges tested for three of the manufacturers. However, in all fairness, they should have pointed out that the nicotine values measured for Johnson Creek refill liquid in Table 4 were very, very close to the label amount, ranging from 100.2% of the label value to 110.8% (18 mg Tennessee Cured was found to contain 19.9 mg/ml.) The statement "Some products were found to contain high concentrations of nicotine when labeled not to contain nicotine" should have been qualified by pointing out that only the CIXI brand contained significant amounts of nicotine in the 0 nicotine product.

Considering the first sentence of the abstract, I find it an egregious omission that the Conclusion section failed to point out that their testing did not detect impurities in the liquid, except for the adulterated products sold by CIXI, and that there were no impurities detected in the vapor of any of the brands tested.

That's my

 

[yvilla]

Elaine, take another look at Table 2. I think that the only carts that may truly have been significantly off are the Cixi carts, especially those labeled to contain no nicotine but that did contain varying amounts.

Otherwise, what this paper shows is the utter absurdity and ignorance of the researchers, not even understanding what the labels purport to convey in the first place. That is, they compare the supposed "Label mg Nicotine per Cartridge" to the "Actual mg Nicotine per Cartridge", when in reality, we all know that filled carts or cartomizers are labeled the same way as bottles are labeled - in mg per ml. So the only way to know how accurate the labeling is in terms of nicotine content is to know the amount of liquid overall in a given cart or cartomizer, and this the idiot researchers did not measure. We also all know that most carts, especially in the kinds of ecigs they bought and tested, do not hold a full ml, but rather 1/3 or 1/2 of a ml. So bottom line, the numbers they found in testing the Njoy and SE carts actually look they would be pretty close to accurate to me!

The researchers only got it right when evaluating the Johnson Creek liquid (Table 4), because there they did know that it was mg per ml.

Final note: Besides showing how ignorant the researchers are, I think this also shows why it would be so much better if everyone switched to the % standard in labeling! It would forestall such misperceptions and misunderstandings that have plagued e-liquid and carts from the start.

 

[DC2]

Otherwise, what this paper shows is the utter absurdity and ignorance of the researchers, not even understanding what the labels purport to convey in the first place. That is, they compare the supposed "Label mg Nicotine per Cartridge" to the "Actual mg Nicotine per Cartridge", when in reality, we all know that filled carts or cartomizers are labeled the same way as bottles are labeled - in mg per ml. So the only way to know how accurate the labeling is in terms of nicotine content is to know the amount of liquid overall in a given cart or cartomizer, and this the idiot researchers did not measure.

That is exactly what I thought while reading Elaine's post, but I hadn't read the study yet so I wasn't sure.

 

[Spazmelda]

Is there anywhere I can get a pdf of this paper? I tried the link posted above, but it only showed me the first page with the rest requiring a subscription.

I've got a Ph.D. in molecular biology and lots of experience reading papers and methods, and I'd love to give the paper a read through and give my opinions.

 

[DC2]

The idea of paying $41.00 to read the details of a government analysis doesn't sit well at all with me.

 

[yvilla]

Spazmelda, pm me your email, and I'll send you the pdf.

 

[rothenbj]

These "impurities" as the FDA scientists call them are not tobacco impurities (perhaps impurities in extracted nicotine), they are the WTAs found in tobacco plants- whole tobacco alkaloids. It has been theorized for years now that what some of us find missing in current nicquid are these WTAs. A few members have been working on creating liquid that would incorporate these alkaloids extracted from tobacco and added to nicquid.

 

[DC2]

These "impurities" as the FDA scientists call them are not tobacco impurities (perhaps impurities in extracted nicotine), they are the WTAs found in tobacco plants- whole tobacco alkaloids. It has been theorized for years now that what some of us find missing in current nicquid are these WTAs. A few members have been working on creating liquid that would incorporate these alkaloids extracted from tobacco and added to nicquid.

Honest question, for fun and speculation...

Who thinks the FDA is aware of the efforts to incorporate these "impurities" in nicquid?
Who thinks the FDA is aware that some tobacco companies are already producing products that purposely include these "impurities"?

I can see them not being aware of the former, but I find it hard to believe they are not aware of the latter.
In fact, I find it pretty much impossible.

 

[cookiebun]

First off, I haven't finished reading this entire thread. I really feel it's important to ask, has anyone bothered to consider how many ecig users consistently or exclusively use prefilled carts or cartomizers? I'd be willing to bet most people don't stick with this stuff for long. They move on to juice vendors who make a better quality and tastier product. What's in the prefilled carts/cartos shouldn't be such a big issues.
Test Dekang Juices, test nicotine base from Box Elder, Extreme Vaping ect. Figure out whats the most popular and test that.
Just a suggestion.

 

[Vocalek]

Excellent catch, Yolanda. See, this is what happens when researchers think they are smarter than consumers and refuse to include them in the process.

And refusing to include consumers in the process is why the entire world of tobacco control has an incomplete understanding about why people smoke (they think we do it to "get high").

 

[Grammie]

@Vocalek .. I always enjoy your posts and you are a very well spoken young woman ..

I believe we are in the Wild Wild West phase of this industry and I call this the Golden Age of the PV .. there is no way, especially with the growth of the product, that regulation / etc, will not step in, sooner than later ..

I applaud you for fighting the good fight .. but I am afraid that a product based on nicotine will, as you say, "they are going to be regulating the product you know and love so tightly" ..

I don't like it any more than anyone else .. however, it appears to be the only path towards any degree of consistency in this industry ..

I don't fret (much) over the quality and ingredients of the liquid I use .. but I do know that I really don't know what a maker puts in it .. and anything that is ingested, in any form, should have at least a certain degree of expected quality ..

Yes, I know we have regular food scares / and nothing is fully safe .. the arguments been beat to death on the forum ..

Uncle Willie, I don't have the time left in my life to wait until the FDA "GETS IT". If I should smoke and wait til the truth comes out I will no doubt die. I choose to at least try to save my life! That's what they'll take away from me and my family if we just let them run rough shod over us. Oh, they'll give (make us PAY) us something but nothing like what most of us need.

I'm not arguing with you, Uncle Willie, but it's time for us all to wake up and make our own choices on what we do know. Vaping for us has to be better than all those extra added chemicals in the real cigarettes. My own health tells me it is tons better.

 

[kristin]

Just looking at what these groups are testing for shows that their whole interest is in the product as a threat to NRT. Not one test from the ANTZ, besides the FDA test, has attempted to show the actual health risks compared to smoking. All of the tests are looking to make the NRTs appear to be safer and more effective. They've tested for nicotine delivery (three times now), accuracy of labeling and defects such as leaking carts. All of these test results are designed to be able to point the public back toward NRTs as if to say "NRT has better labeling, no leaking and consistency." The only reason I can think of to be so preoccupied with these things over actual discovery of potential SERIOUS health risks (they obviously know the chance of finding anything significant and consistent over different brands is slim to none) or testing health risks compared to smoking is fear of competition, not fear for public health.

 

[Spazmelda]

I've started reading through the paper, focusing mostly on the nicotine level determination for now. I also had my husband look over it briefly as he is a chemist and does all that chromatography stuff (HPLC etc...)

The accuracy and precision of the brands other than Johnson Creek were really pretty abysmal and do point to false advertising and sloppy technique and quality control of those companies. The issue of whether the carto labels were indicating mgs or mgs/ml doesn't adequately explain the variances between samples of the same strength nic solution. I mean, even if the cartos were actually 11 mg/*ML* they are still not even in the right ball park in many cases. And, I've thought this since I first started looking at and buying cartos... if a carto says 18 mg it should have 18 mg in it. If it's really 18 mg/ml it should SAY 18 mg/ml. Labeling as 18 mg implies that there is a total of 18 mg of nicotine present.

The fact that nicotine was present in some of the caros labeled as 0 is pretty bad. All of this points toward false advertising, and having high levels of nic in some of the 0 nic samples is not good at all. I'd be very interested in seeing results like this from a couple of the American e-juice suppliers, and I suspect that their accuracy would be much better. I think if you are in the e-juice business you probably should be doing some spot checking with an independent lab as part of your quality control practices.

Johnson Creek should be commended for their extremely accurate nic concentrations. My husband was very impressed with their % of label numbers. The authors played that part down, it seems.

I haven't gotten around to looking at the parts of the paper dealing with impurities, but I do wish they'd have included an analog in that test. My husband says he can look at the 'sheets' (or something) to see what sort of levels are generally considered acceptable for each compound. I'll see if I can get him to do that, but he's really busy at work (he's actually going to present something to the FDA next week, lol, but not having anything to do with e-cigs).

 

[kristin]

Thanks for your observations so far, Spazmelda. The issue of quality control and accurate labeling have always been of concern in our community. It was pretty much a given that as e-cigarettes became more popular, shady manufacturers would start trying to increase their ROI by cutting corners. It's one reason we've been calling for a decent e-cigarette association to initiate some standards.

It would be very interesting to hear what those levels of "impurities" really mean when translated into actual health risks. The tactic of bringing up "impurities" while not giving any actual comparison or indication of health risks is suspiciously similar to the FDA claiming e-cigarettes have carcinogens and toxic chemicals "also found in antifreeze" without qualifying that the actual health risks of the levels found were negligible to non-existent.

 

[yvilla]

The accuracy and precision of the brands other than Johnson Creek were really pretty abysmal and do point to false advertising and sloppy technique and quality control of those companies. The issue of whether the carto labels were indicating mgs or mgs/ml doesn't adequately explain the variances between samples of the same strength nic solution. I mean, even if the cartos were actually 11 mg/*ML* they are still not even in the right ball park in many cases. And, I've thought this since I first started looking at and buying cartos... if a carto says 18 mg it should have 18 mg in it. If it's really 18 mg/ml it should SAY 18 mg/ml. Labeling as 18 mg implies that there is a total of 18 mg of nicotine present.

That's why a change to the percentage standard in labeling is so necessary. That is, 18 mg eliquid should actually be labeled as having 1.8% nicotine content. It is only relatively recently that some eliquid sellers, notably in the US like Puresmoker, have switched to such percentage labeling. But, it is assuredly true that these studied carts were labeled with a given quantity of nicotine per mg, and NOT per cart. It has always been that way.

So when you consider that most of the Njoy and SE carts these researchers looked at most likely did have only from 1/3 to 1/2 ml eliquid content each, the results they found really were not so far off. Really - take another look at the SE and Njoy results from Table 2 as copied out by Vocalek above (my comments in blue):

Smoking Everywhere
0 mg. cartridges - ranged from 0.0 to 0.1 mg.
6 mg. cartridges - ranged from 1.0 to 2.7 mg. (6 / 3 = 2)
11 mg. cartridges - ranged from 2.7 to 5.2 mg. (11 / 3 = 3.6; 11 / 2 = 5.5)
16 mg. cartridges - ranged from 4.2 to 6.0 mg. (16 / 3 = 5.3)

NJOY
6 mg. cartridge - 5.2 mg. (this does seem pretty far off, for a cart with less than 1 ml eliquid)
12 mg. cartridges - ranged from 4.3 to 5.3 mg. (12 / 3 = 4)
18 mg. cartridge - 6.8 mg. (18 / 3 = 6)

The Cixi results do seem off altogether, however, as I acknowledged before

I haven't gotten around to looking at the parts of the paper dealing with impurities, but I do wish they'd have included an analog in that test.

If you looked at it only quickly you might have just missed it, Spazmelda. For they DO compare regular cigarettes with the tested eliquid in this part of the paper dealing with "nicotine related impurities". Look at Table 6 at the top of page 15 of the PDF. It's quite instructive! (But as noted by rothenbj above, these "impurities" are not considered impurities by some).

What this study does not do at all is look at or for the known carcinogens and the worst of the toxins found in cigarette smoke, much less compare quantities found between cigarettes and eliquids.

 

[kristin]

If you looked at it only quickly you might have just missed it, Spazmelda. For they DO compare regular cigarettes with the tested eliquid in this part of the paper dealing with "nicotine related impurities". Look at Table 6 at the top of page 15 of the PDF. It's quite instructive! (But as noted by rothenbj above, these "impurities" are not considered impurities by some).

What this study does not do at all is look at or for the known carcinogens and the worst of the toxins found in cigarette smoke, much less compare quantities found between cigarettes and eliquids.

Thanks, Yolanda - I missed that, too. What does "ND" mean on the chart? None/Not detected? I wonder what the results were for the other 3 brands and why they aren't included?

 

[yvilla]

Yep, ND means not detected. Also look at Figure 7 - but pay careful attention to the numbers along the vertical axis. They make it look like the same amounts found, because the visual spike is the same height - but the amount at the top of the spike in the graph for the cigarettes is 100, and the amount for the e-cigarette is 5.

I wondered about them only including the Cixi cart in Table 7 too. It's probably because the other two brands were also all ND results.

 

[Spazmelda]

That's why a change to the percentage standard in labeling is so necessary. That is, 18 mg eliquid should actually be labeled as having 1.8% nicotine content. It is only relatively recently that some eliquid sellers, notably in the US like Puresmoker, have switched to such percentage labeling. But, it is assuredly true that these studied carts were labeled with a given quantity of nicotine per mg, and NOT per cart. It has always been that way.

You have more experience with this sort of thing than I do, but I do know I ordered some cartos that were labeled as '18 mg' or '12 mg' (both unbranded as far as I know though). Looking at both Smoke Anywhere and NJOY's websites I do see that they are labeled with % or mg/ml (or both in the case of Smoke Anywhere). So if they were indeed labeled that way, then the FDA researchers really screwed that one up, and the only way to know for sure would have been to measure the volume of liquid, which they didn't do. Hopefully the e-cig companies in question will address that issue with letters to the journal. The variation in total nic and nic in 0 mg cartos is still worrisome, mostly in the case of CIXA.

I did miss the analysis of the analog. Very interesting.