Introduction
Heroin (diacetylmorphine) is a synthetic opioid available on most darknet markets. In Europe, it is almost exclusively sold as heroin #3, a brown powder containing diacetylmorphine (DAM) as water-insoluble base. For heroin users, it is very difficult to make an objective judgment about the quality of the heroin they bought because of their individual opioid tolerance, the varying quality of the purchased products and not at least because of the incorrect or missing information about the purity of the products given by the vendors. Also, drug checking services are not available in many countries, yet. In order to contribute to safer use of heroin as well as shedding some more light on the quality of the heroin that vendors are selling on the darknet, a relatively simple and reliable method for estimation of the DAM content of heroin #3 was developed.
Methods describing the purification of heroin have already been published, e. g. by Steve J. Quest on the Erowid website (1). This frequently cited protocol does not work for the desired purpose because of unsuitable stoichiometry of the chemicals in a certain step of the procedure (see below). Therefore, the method published on Erowid was modified at the critical steps. The vast majority of adulterants and impurities should be removed during the purification process yielding a relatively pure sterile product with an at least calculable DAM content that can directly be used for consumption. The whole procedure takes about 5 hours including sample incubation and drying times. Principally, it can be performed by any interested non-scientist who is willing to invest some time in learning safe handling of the used chemicals.
The method was tested multiple times with heroin #3 obtained from different European vendors (all samples were measured at least in duplicate). The essential conclusions of these analyses are summarized at the end of the article.
Procedure’s limitations
The protocol enriches alkaloids, including the target substance DAM. As already stated on the Erowid website, alkaloids that are chemically related to DAM, p. e. monoacetylmorphine, morphine, codeine or thebaine might not or not completely be eliminated when present in the sample.
Heroin is commonly cut with caffeine and paracetamol (2). Because of their bad solubility in diethyl ether, these adulterants are most likely eliminated by this protocol.
Safety notice regarding fentanyl
Fentanyl is a highly potent synthetic opioid (50 to 100-fold stronger than morphine) with a relatively short serum half-life that is locally used as adulterant for heroin or even sold as heroin #4 (DAM hydrochloride), especially in the USA (3,4). Because of its higher potency, the presence of fentanyl significantly increases the risk of an unintended deadly opioid overdose. Due to missing experimental data, it cannot be excluded that the described method enriches fentanyl when present in the processed heroin sample. Consequently, it is strongly recommended to test the purified product for the presence of fentanyl by using urine test stripes.
Safe handling of chemicals
The following described procedure uses highly aggressive, corrosive, and volatile chemicals. For every chemical, safety data sheets (SDS) are available that are provided by the manufacturer or reseller of the product. They can be downloaded from the internet. It is strongly recommended to carefully read these SDS and follow the safety instructions therein.
Diethyl ether tends to form explosive peroxides with oxygen, but most diethyl ether products are stabilized by addition of small amounts of antioxidants. As long as diethyl ether is not distilled and handled and stored in small quantities, it is relatively safe to work with. But it should not be stored longer than necessary because the risk of peroxide formation increases over time.
Materials
0,5 g heroin #3
hydrochloric acid (HCl, 37%)
distilled water (H2O)
ammonia solution 25 %
diethyl ether
ethanol (96 % or 99,8%)
glass Petri dish or evaporating basin (capacity minimum 30 ml)
polypropylene (PP) test tubes 1,5 ml (easy cap), 15 ml (screw cap), 50 ml (screw cap)
glass and micro tip pipettes (100 µl – 20 ml)
spatula
laboratory scale (d= 0,001 g, max. 100 g)
universal indicator paper pH 1-14
micro centrifuge
personal protective equipment according to SDS (gloves, safety glasses, lab coat)
Extraction of heroin and determination of DAM content
Place 0,5 g of heroin #3 in a 15 ml PP screw cap test tube and add 200 µl HCl. The sample should be soaked completely with acid. In this step the water-insoluble DAM base of the heroin #3 is converted to water-soluble DAM hydrochloride (DAM-HCl). Next, add 5 ml H2O and mix thoroughly. Warm the sample a water bath (40-60 °C) and continue mixing until all soluble substances are solved. Depending on the purity of the heroin sample, this steps typically yields a more or less clear yellow to light brown solution containing a black-brown insoluble, sticky precipitate. The pH value of the solution is very low, about pH 1-2.
In the next step, all insoluble substances are separated from the acidic solution. This works best by centrifugation (aliquot the 5 ml into four 1,5 ml PP reaction tubes and centrifuge in a micro centrifuge). Filtration or gravitational settling should also work (not tested for this protocol). Transfer the supernatant into a fresh 15 ml PP screw cap test tube. The obtained solution is yellow to brown and should be absolutely clear for an optimal result.
In the following step, the water-soluble DAM-HCl is reconverted to water-insoluble DAM base by addition of approximately 300 µl of ammonia solution. Add the ammonia solution drop-wise while gently shaking the reaction tube until no more precipitate is formed. The solution should be turbid/milky now, the formed precipitate is white to gray and sticky. When high quality heroin is used, the precipitate forms a big sticky lump, low quality heroin rather yields a turbid suspension. The pH value should be 9 or higher.
Next, liquid-liquid extraction with diethyl ether is used to isolate the DAM base from the aqueous phase. For yielding a maximum of DAM base, repeated extraction with small quantities of diethyl ether is more effective than performing only one extraction with a big volume of diethyl ether (compare to the protocol on Erowid). Add 5 ml of diethyl ether to the solution and mix gently by inverting the tube several times. Let the tube stand until the phases are completely separated. Diethyl ether won’t mix with the aqueous phase but will form a separate layer on top. Isolate the upper diethyl ether phase and place it into a fresh 50 ml PP screw cap reaction tube. Diethyl ether is highly volatile and the probe should not stand for a longer time in this working step, because the DAM base tends to precipitate from the ether phase, especially when high quality heroin #3 is processed. When precipitation happens, it is difficult to redissolve the DAM base because of the low boiling point of diethyl ether. Redissolution can be achieved by adding more diethyl ether and very careful and gently warming to max. 30 °C (boiling point of diethyl ether is about 35 °C). Repeat the extraction with 5 ml diethyl ether portions two more times and combine the extracts in a 50 ml PP screw cap reaction tube. The obtained extract typically has a light yellow to orange color and should be clear without any precipitate.
The diethyl ether extract is now washed two times with H2O. Add 10 ml of H2O to the ether extract and gently invert the tube several times. Let the mixture stand for about a minute until the phases are separated completely. Remove the lower, aqueous phase with a pipette and discard it. Repeat this washing step one more time.
Take a clean Petri dish or evaporating basin and determine its empty mass by weighing. Document the value. Transfer the diethyl ether extract into the Petri dish and rinse the 50 ml PP reaction tube with a small amount of diethyl ether in order to transfer all of your product into the Petri dish. Let the diethyl ether evaporate at room temperature at a well ventilated place (p. e. window-sill with open window). Evaporation will happen within a few minutes due to the high vapor pressure of diethyl ether. Usually, a white precipitate will form at the end of the diethyl ether evaporation. This precipitate is mostly DAM base. Also, there will be some water drops left because of the prior washing step with H2O. When only the water drops are left and the extract does not smell like diethyl ether anymore, the Petri dish can be placed into an oven (40 °C) to speed up evaporation of the residual water. The extract will turn glassy and more transparent during warming with white to light pink or orange crystals, especially around the areas where the water drops were located. Dry the extract until the mass reaches a constant value. Document the mass of the Petri dish containing the heroin extract.
Although the yielded extract is mostly DAM base, it also contains other alkaloids of the poppy plant and the heroin production process, like monoacetylmorphine, morphine, codeine, thebaine and traces of residual water (because no desiccator is used for drying). The amount of DAM base in this mixture is estimated as 80% in this protocol (not validated experimentally).
The DAM content of the extract is calculated as follows:
mass Petri dish with extract after drying (g) - mass empty Petri dish (g) = mass heroin #3 extract (g)
estimated DAM content of heroin #3 sample (g) = mass heroin #3 extract (g) * 0,8
mass heroin #3 extract (g) / mass heroin #3 used for purification (g) * 100 = extractable substances of heroin #3 sample (%)
estimated DAM content of heroin #3 (%) = extractable substances of the heroin #3 sample (%) * 0,8
Preparing a DAM-HCl solution
The second part of this protocol can be used to prepare a consumable heroin solution with reproducible DAM-HCl concentration. From now on, this protocol significantly differs from the method published on the Erowid website. Although conversion of DAM base dissolved in diethyl ether to DAM-HCl and simultaneous extraction into the lower aqueous phase by addition of water and HCl is possible, the described procedure is unsuitable for the production of a consumable heroin solution because of inappropriate stoichiometry of the applied chemicals. In the method on the Erowid website, an enormous amount of HCl is added that has subsequently to be neutralized by addition of stoichiometric amounts of Na2CO3 (washing soda). A relatively simple calculation of the applied mass concentrations revealed that in Erowid’s protocol, around 2,5 g NaCl (table salt) are formed. This NaCl is declared as a by-product in the protocol but in fact, NaCl is the main product at the end of the neutralization of HCl. For instance, when purifying 1 g heroin with 26 % DAM with the Erowid method, the final DAM concentration among the 2,5 g NaCl formed would only be approximately 10 %. Compared to the original substance with 26 % DAM this would be a reduction in DAM concentration and therefore not expedient at all for the desired purpose. I checked this experimentally just for fun and actually yielded almost exactly the calculated amount of NaCl.
In order to convert the DAM base included in the dried extract to an injectable form, another conversion into DAM-HCl is necessary. Mix 6 ml of ethanol with 520 µl diluted HCl (1:10 with H2O) and mix thoroughly. Disperse the dried DAM base residue in the Petri dish with small portions of this solvent mixture. A spatula can be used to scratch all substance off the glass. The DAM base will not dissolve immediately but will form a light yellow to orange suspension with white precipitate (nearly pure DAM base). Transfer all of this precipitate/suspension into a fresh 15 ml PP screw cap reaction tube. Rinse the Petri dish with small portions of the ethanol/HCl mixture in order to transfer all undissolved DAM base. Warm the 15 ml PP screw cap reaction tube in a water bath (50 °C) until a clear solution is obtained (light yellow to orange color). Place a tiny drop of this solution onto a glass surface (e. g. Petri dish) and let it dry. When the DAM base of the solution has not been turned into DAM-HCl completely, a white opaque residue/precipitate will remain on the glass surface. The pH value of the solution is relatively high (pH 5-6). Add another tiny drop (50 µl) of 1:10 diluted HCl to the solution and repeat the test. When a stoichiometric amount of HCl is added, the drop on the glass plate will behave differently. The residue is absolutely clear and almost invisible. Also, the pH value of the solution is lower now (pH 2-4). Depending on the DAM content of the used heroin 0-400 µl of 1:10 diluted HCl have to be added. When DAM content is very low, the HCl amount in the ethanol/HCl solution must be reduced. This procedure is kind of a titration and ensures that all DAM base is converted to DAM-Hcl. At the same time it is prevented that an excess of HCl is added to the mixture.
Transfer the dissolved DAM-HCl in ethanol into a fresh Petri dish. Rinse the 15 ml PP reaction tube three times with 1 ml ethanol and pool this with the extract in the Petri dish. Let the solvent evaporate completely. Evaporation can be enhanced by moderate heating in an oven (40 °C). The obtained residue is typically completely clear and colorless, like glass, sometimes with some white crystals.
Because the mass of the extracted alkaloids was gravimetrically determined, a heroin solution with defined concentration (p. e. 10 mg/ml) can be obtained by addition of a calculated volume of H2O (normally 8-25 ml). The addition of water yields a more or less turbid suspension. As before, rinse the Petri dish with a spatula and small fractions of H2O and combine these in a 50 ml PP screw cap reaction tube. Place this into a cooking water bath (5-10 min). Some turbidity will remain after cooking. Sterilize the solution with a syringe driven filter (polyethersulfone, PES, or polyvinylidene fluoride PVDF, 0,22 µm) and aliquot in sterile 1,5 ml PP reaction tubes. Control the pH value of the solution, it should be 6-7. The solution is stable at room temperature for at least 15 days (5). For longer storage, it should be stored at -20 °C in a fridge. After thawing, heat the probe to ensure all substances are completely redissolved.
Depending on the amount of H2O used for dissolving the purified DAM-HCl in the last reaction step, the obtained solution has a high concentration of DAM-HCl. All calculations should be done very carefully to avoid accidental overdosing. When using heroin for the first time, better start with a very low dose not exceeding 5 mg (6).
Results of analyses of heroin #3 samples
Analyses of heroin #3 samples (n=45) (25-80 €/g) obtained from 7 different European darknet vendors by the described method resulted in following conclusions:
- in average, the samples contained 55-60 % extractable substance (minimum 14 %, maximum 77 %)
- most samples had a DAM content between 40 % and 50 % (minimum 10 %, maximum 63 %)
- this finding is consistent with an article published on dread (7)
- it is assumed that all samples contained adulterants, most likely caffeine and paracetamol (2)
- fentanyl was not detected in any of the samples (testing was performed randomly with urine test stripes), this is also consistent with the findings published in (2)
- only one vendor indicated a realistic DAM content of his product
- there was no correlation between price and DAM content, consequently expensive heroin did not have a higher DAM content
- the best heroin #3 tested so far contained more than 60% DAM and costed 25 €/g (vendor misterrx on Alphabay market)
- more than once, heroin with a higher DAM content was sent after my first order, while in the following orders, I was provided with heroin #3 with a lower DAM content
- the average weight of the delivered products was acceptable (+/- 10 % of the ordered quantity)
Discussion
I am not at all satisfied with the estimation of the DAM content of the extract. Although, I assume that this is a rather conservative and also a realistic value at least for high quality heroin, it would be very helpful to investigate the components of the obtained DAM-HCl solution by HPLC and GC/MS in a drug checking lab. Maybe somebody is interested in doing that and add the information here.
Regarding the liquid-liquid extraction, I tested MTBE as an alternative to diethyl ether, which also worked. MTBE does not form explosive peroxides with oxygen, but is slightly more toxic than diethyl ether. Other possible alternatives for extraction are petrol ether and n-hexane. Maybe somebody has already tested these solvents and can add some information about their applicability. Sometimes the phases in the liquid-liquid extraction do not separate very well. This might be improved by addition of NaCl.
In the last working step when DAM-HCl is dissolved in H2O, small amounts of an insoluble substance can be observed. This is very likely not DAM base because addition of more acid does not dissolve this substance. Addition of propylene glycol does, so it is a hydrophobic substance. Does anybody have an idea about the identity of this substance?
Finally, it is really important to investigate whether fentanyl is enriched or eliminated by the described method.
Author’s comment
I believe in freedom of speech and autonomy and think that the restrictive drug politics and stigmatization of drug users in my home country and many other countries of the world violate human rights and in sum damage society. The discrimination rather has historical and political reasons (8) and in my opinion is not based on medical, ethical or humanistic considerations in many aspects and that is why it is deficient and inacceptable. Because we still have a long way to go in this field, I decided to write this article and hope that it helps people in terms of responsible drug use and harm reduction.
Peace, love, empathy,
Ana
References
1 https://erowid.org/chemicals/heroin/heroin_info5.shtml
2 https://doi.org/10.1186/s12954-021-00544-x
3 https://www.rollingstone.com/cultur...-opioid-heroin-epidemic-getting-worse-717847/
4 https://doi.org/10.1016/j.drugpo.2017.06.010
5 https://doi.org/10.1093/ajhp/47.2.377
6 https://psychonautwiki.org/wiki/Diacetylmorphine
7 http://dreadytofatroptsdj6io7l3xptbet6onoyno2yv7jicoxknyazubrad.onion/post/b23ff4e3328b38c8f23f
8 https://doi.org/10.1186/s12954-022-00593-w
Heroin (diacetylmorphine) is a synthetic opioid available on most darknet markets. In Europe, it is almost exclusively sold as heroin #3, a brown powder containing diacetylmorphine (DAM) as water-insoluble base. For heroin users, it is very difficult to make an objective judgment about the quality of the heroin they bought because of their individual opioid tolerance, the varying quality of the purchased products and not at least because of the incorrect or missing information about the purity of the products given by the vendors. Also, drug checking services are not available in many countries, yet. In order to contribute to safer use of heroin as well as shedding some more light on the quality of the heroin that vendors are selling on the darknet, a relatively simple and reliable method for estimation of the DAM content of heroin #3 was developed.
Methods describing the purification of heroin have already been published, e. g. by Steve J. Quest on the Erowid website (1). This frequently cited protocol does not work for the desired purpose because of unsuitable stoichiometry of the chemicals in a certain step of the procedure (see below). Therefore, the method published on Erowid was modified at the critical steps. The vast majority of adulterants and impurities should be removed during the purification process yielding a relatively pure sterile product with an at least calculable DAM content that can directly be used for consumption. The whole procedure takes about 5 hours including sample incubation and drying times. Principally, it can be performed by any interested non-scientist who is willing to invest some time in learning safe handling of the used chemicals.
The method was tested multiple times with heroin #3 obtained from different European vendors (all samples were measured at least in duplicate). The essential conclusions of these analyses are summarized at the end of the article.
Procedure’s limitations
The protocol enriches alkaloids, including the target substance DAM. As already stated on the Erowid website, alkaloids that are chemically related to DAM, p. e. monoacetylmorphine, morphine, codeine or thebaine might not or not completely be eliminated when present in the sample.
Heroin is commonly cut with caffeine and paracetamol (2). Because of their bad solubility in diethyl ether, these adulterants are most likely eliminated by this protocol.
Safety notice regarding fentanyl
Fentanyl is a highly potent synthetic opioid (50 to 100-fold stronger than morphine) with a relatively short serum half-life that is locally used as adulterant for heroin or even sold as heroin #4 (DAM hydrochloride), especially in the USA (3,4). Because of its higher potency, the presence of fentanyl significantly increases the risk of an unintended deadly opioid overdose. Due to missing experimental data, it cannot be excluded that the described method enriches fentanyl when present in the processed heroin sample. Consequently, it is strongly recommended to test the purified product for the presence of fentanyl by using urine test stripes.
Safe handling of chemicals
The following described procedure uses highly aggressive, corrosive, and volatile chemicals. For every chemical, safety data sheets (SDS) are available that are provided by the manufacturer or reseller of the product. They can be downloaded from the internet. It is strongly recommended to carefully read these SDS and follow the safety instructions therein.
Diethyl ether tends to form explosive peroxides with oxygen, but most diethyl ether products are stabilized by addition of small amounts of antioxidants. As long as diethyl ether is not distilled and handled and stored in small quantities, it is relatively safe to work with. But it should not be stored longer than necessary because the risk of peroxide formation increases over time.
Materials
0,5 g heroin #3
hydrochloric acid (HCl, 37%)
distilled water (H2O)
ammonia solution 25 %
diethyl ether
ethanol (96 % or 99,8%)
glass Petri dish or evaporating basin (capacity minimum 30 ml)
polypropylene (PP) test tubes 1,5 ml (easy cap), 15 ml (screw cap), 50 ml (screw cap)
glass and micro tip pipettes (100 µl – 20 ml)
spatula
laboratory scale (d= 0,001 g, max. 100 g)
universal indicator paper pH 1-14
micro centrifuge
personal protective equipment according to SDS (gloves, safety glasses, lab coat)
Extraction of heroin and determination of DAM content
Place 0,5 g of heroin #3 in a 15 ml PP screw cap test tube and add 200 µl HCl. The sample should be soaked completely with acid. In this step the water-insoluble DAM base of the heroin #3 is converted to water-soluble DAM hydrochloride (DAM-HCl). Next, add 5 ml H2O and mix thoroughly. Warm the sample a water bath (40-60 °C) and continue mixing until all soluble substances are solved. Depending on the purity of the heroin sample, this steps typically yields a more or less clear yellow to light brown solution containing a black-brown insoluble, sticky precipitate. The pH value of the solution is very low, about pH 1-2.
In the next step, all insoluble substances are separated from the acidic solution. This works best by centrifugation (aliquot the 5 ml into four 1,5 ml PP reaction tubes and centrifuge in a micro centrifuge). Filtration or gravitational settling should also work (not tested for this protocol). Transfer the supernatant into a fresh 15 ml PP screw cap test tube. The obtained solution is yellow to brown and should be absolutely clear for an optimal result.
In the following step, the water-soluble DAM-HCl is reconverted to water-insoluble DAM base by addition of approximately 300 µl of ammonia solution. Add the ammonia solution drop-wise while gently shaking the reaction tube until no more precipitate is formed. The solution should be turbid/milky now, the formed precipitate is white to gray and sticky. When high quality heroin is used, the precipitate forms a big sticky lump, low quality heroin rather yields a turbid suspension. The pH value should be 9 or higher.
Next, liquid-liquid extraction with diethyl ether is used to isolate the DAM base from the aqueous phase. For yielding a maximum of DAM base, repeated extraction with small quantities of diethyl ether is more effective than performing only one extraction with a big volume of diethyl ether (compare to the protocol on Erowid). Add 5 ml of diethyl ether to the solution and mix gently by inverting the tube several times. Let the tube stand until the phases are completely separated. Diethyl ether won’t mix with the aqueous phase but will form a separate layer on top. Isolate the upper diethyl ether phase and place it into a fresh 50 ml PP screw cap reaction tube. Diethyl ether is highly volatile and the probe should not stand for a longer time in this working step, because the DAM base tends to precipitate from the ether phase, especially when high quality heroin #3 is processed. When precipitation happens, it is difficult to redissolve the DAM base because of the low boiling point of diethyl ether. Redissolution can be achieved by adding more diethyl ether and very careful and gently warming to max. 30 °C (boiling point of diethyl ether is about 35 °C). Repeat the extraction with 5 ml diethyl ether portions two more times and combine the extracts in a 50 ml PP screw cap reaction tube. The obtained extract typically has a light yellow to orange color and should be clear without any precipitate.
The diethyl ether extract is now washed two times with H2O. Add 10 ml of H2O to the ether extract and gently invert the tube several times. Let the mixture stand for about a minute until the phases are separated completely. Remove the lower, aqueous phase with a pipette and discard it. Repeat this washing step one more time.
Take a clean Petri dish or evaporating basin and determine its empty mass by weighing. Document the value. Transfer the diethyl ether extract into the Petri dish and rinse the 50 ml PP reaction tube with a small amount of diethyl ether in order to transfer all of your product into the Petri dish. Let the diethyl ether evaporate at room temperature at a well ventilated place (p. e. window-sill with open window). Evaporation will happen within a few minutes due to the high vapor pressure of diethyl ether. Usually, a white precipitate will form at the end of the diethyl ether evaporation. This precipitate is mostly DAM base. Also, there will be some water drops left because of the prior washing step with H2O. When only the water drops are left and the extract does not smell like diethyl ether anymore, the Petri dish can be placed into an oven (40 °C) to speed up evaporation of the residual water. The extract will turn glassy and more transparent during warming with white to light pink or orange crystals, especially around the areas where the water drops were located. Dry the extract until the mass reaches a constant value. Document the mass of the Petri dish containing the heroin extract.
Although the yielded extract is mostly DAM base, it also contains other alkaloids of the poppy plant and the heroin production process, like monoacetylmorphine, morphine, codeine, thebaine and traces of residual water (because no desiccator is used for drying). The amount of DAM base in this mixture is estimated as 80% in this protocol (not validated experimentally).
The DAM content of the extract is calculated as follows:
mass Petri dish with extract after drying (g) - mass empty Petri dish (g) = mass heroin #3 extract (g)
estimated DAM content of heroin #3 sample (g) = mass heroin #3 extract (g) * 0,8
mass heroin #3 extract (g) / mass heroin #3 used for purification (g) * 100 = extractable substances of heroin #3 sample (%)
estimated DAM content of heroin #3 (%) = extractable substances of the heroin #3 sample (%) * 0,8
Preparing a DAM-HCl solution
The second part of this protocol can be used to prepare a consumable heroin solution with reproducible DAM-HCl concentration. From now on, this protocol significantly differs from the method published on the Erowid website. Although conversion of DAM base dissolved in diethyl ether to DAM-HCl and simultaneous extraction into the lower aqueous phase by addition of water and HCl is possible, the described procedure is unsuitable for the production of a consumable heroin solution because of inappropriate stoichiometry of the applied chemicals. In the method on the Erowid website, an enormous amount of HCl is added that has subsequently to be neutralized by addition of stoichiometric amounts of Na2CO3 (washing soda). A relatively simple calculation of the applied mass concentrations revealed that in Erowid’s protocol, around 2,5 g NaCl (table salt) are formed. This NaCl is declared as a by-product in the protocol but in fact, NaCl is the main product at the end of the neutralization of HCl. For instance, when purifying 1 g heroin with 26 % DAM with the Erowid method, the final DAM concentration among the 2,5 g NaCl formed would only be approximately 10 %. Compared to the original substance with 26 % DAM this would be a reduction in DAM concentration and therefore not expedient at all for the desired purpose. I checked this experimentally just for fun and actually yielded almost exactly the calculated amount of NaCl.
In order to convert the DAM base included in the dried extract to an injectable form, another conversion into DAM-HCl is necessary. Mix 6 ml of ethanol with 520 µl diluted HCl (1:10 with H2O) and mix thoroughly. Disperse the dried DAM base residue in the Petri dish with small portions of this solvent mixture. A spatula can be used to scratch all substance off the glass. The DAM base will not dissolve immediately but will form a light yellow to orange suspension with white precipitate (nearly pure DAM base). Transfer all of this precipitate/suspension into a fresh 15 ml PP screw cap reaction tube. Rinse the Petri dish with small portions of the ethanol/HCl mixture in order to transfer all undissolved DAM base. Warm the 15 ml PP screw cap reaction tube in a water bath (50 °C) until a clear solution is obtained (light yellow to orange color). Place a tiny drop of this solution onto a glass surface (e. g. Petri dish) and let it dry. When the DAM base of the solution has not been turned into DAM-HCl completely, a white opaque residue/precipitate will remain on the glass surface. The pH value of the solution is relatively high (pH 5-6). Add another tiny drop (50 µl) of 1:10 diluted HCl to the solution and repeat the test. When a stoichiometric amount of HCl is added, the drop on the glass plate will behave differently. The residue is absolutely clear and almost invisible. Also, the pH value of the solution is lower now (pH 2-4). Depending on the DAM content of the used heroin 0-400 µl of 1:10 diluted HCl have to be added. When DAM content is very low, the HCl amount in the ethanol/HCl solution must be reduced. This procedure is kind of a titration and ensures that all DAM base is converted to DAM-Hcl. At the same time it is prevented that an excess of HCl is added to the mixture.
Transfer the dissolved DAM-HCl in ethanol into a fresh Petri dish. Rinse the 15 ml PP reaction tube three times with 1 ml ethanol and pool this with the extract in the Petri dish. Let the solvent evaporate completely. Evaporation can be enhanced by moderate heating in an oven (40 °C). The obtained residue is typically completely clear and colorless, like glass, sometimes with some white crystals.
Because the mass of the extracted alkaloids was gravimetrically determined, a heroin solution with defined concentration (p. e. 10 mg/ml) can be obtained by addition of a calculated volume of H2O (normally 8-25 ml). The addition of water yields a more or less turbid suspension. As before, rinse the Petri dish with a spatula and small fractions of H2O and combine these in a 50 ml PP screw cap reaction tube. Place this into a cooking water bath (5-10 min). Some turbidity will remain after cooking. Sterilize the solution with a syringe driven filter (polyethersulfone, PES, or polyvinylidene fluoride PVDF, 0,22 µm) and aliquot in sterile 1,5 ml PP reaction tubes. Control the pH value of the solution, it should be 6-7. The solution is stable at room temperature for at least 15 days (5). For longer storage, it should be stored at -20 °C in a fridge. After thawing, heat the probe to ensure all substances are completely redissolved.
Depending on the amount of H2O used for dissolving the purified DAM-HCl in the last reaction step, the obtained solution has a high concentration of DAM-HCl. All calculations should be done very carefully to avoid accidental overdosing. When using heroin for the first time, better start with a very low dose not exceeding 5 mg (6).
Results of analyses of heroin #3 samples
Analyses of heroin #3 samples (n=45) (25-80 €/g) obtained from 7 different European darknet vendors by the described method resulted in following conclusions:
- in average, the samples contained 55-60 % extractable substance (minimum 14 %, maximum 77 %)
- most samples had a DAM content between 40 % and 50 % (minimum 10 %, maximum 63 %)
- this finding is consistent with an article published on dread (7)
- it is assumed that all samples contained adulterants, most likely caffeine and paracetamol (2)
- fentanyl was not detected in any of the samples (testing was performed randomly with urine test stripes), this is also consistent with the findings published in (2)
- only one vendor indicated a realistic DAM content of his product
- there was no correlation between price and DAM content, consequently expensive heroin did not have a higher DAM content
- the best heroin #3 tested so far contained more than 60% DAM and costed 25 €/g (vendor misterrx on Alphabay market)
- more than once, heroin with a higher DAM content was sent after my first order, while in the following orders, I was provided with heroin #3 with a lower DAM content
- the average weight of the delivered products was acceptable (+/- 10 % of the ordered quantity)
Discussion
I am not at all satisfied with the estimation of the DAM content of the extract. Although, I assume that this is a rather conservative and also a realistic value at least for high quality heroin, it would be very helpful to investigate the components of the obtained DAM-HCl solution by HPLC and GC/MS in a drug checking lab. Maybe somebody is interested in doing that and add the information here.
Regarding the liquid-liquid extraction, I tested MTBE as an alternative to diethyl ether, which also worked. MTBE does not form explosive peroxides with oxygen, but is slightly more toxic than diethyl ether. Other possible alternatives for extraction are petrol ether and n-hexane. Maybe somebody has already tested these solvents and can add some information about their applicability. Sometimes the phases in the liquid-liquid extraction do not separate very well. This might be improved by addition of NaCl.
In the last working step when DAM-HCl is dissolved in H2O, small amounts of an insoluble substance can be observed. This is very likely not DAM base because addition of more acid does not dissolve this substance. Addition of propylene glycol does, so it is a hydrophobic substance. Does anybody have an idea about the identity of this substance?
Finally, it is really important to investigate whether fentanyl is enriched or eliminated by the described method.
Author’s comment
I believe in freedom of speech and autonomy and think that the restrictive drug politics and stigmatization of drug users in my home country and many other countries of the world violate human rights and in sum damage society. The discrimination rather has historical and political reasons (8) and in my opinion is not based on medical, ethical or humanistic considerations in many aspects and that is why it is deficient and inacceptable. Because we still have a long way to go in this field, I decided to write this article and hope that it helps people in terms of responsible drug use and harm reduction.
Peace, love, empathy,
Ana
References
1 https://erowid.org/chemicals/heroin/heroin_info5.shtml
2 https://doi.org/10.1186/s12954-021-00544-x
3 https://www.rollingstone.com/cultur...-opioid-heroin-epidemic-getting-worse-717847/
4 https://doi.org/10.1016/j.drugpo.2017.06.010
5 https://doi.org/10.1093/ajhp/47.2.377
6 https://psychonautwiki.org/wiki/Diacetylmorphine
7 http://dreadytofatroptsdj6io7l3xptbet6onoyno2yv7jicoxknyazubrad.onion/post/b23ff4e3328b38c8f23f
8 https://doi.org/10.1186/s12954-022-00593-w
