I normally don’t talk or in this case post on forums much but I have used a lot of information from this site, which has been very helpful. This posting is more of me giving back for all the useful information.
To start I conducted a number of experiments with acacia confusa which was offshoot from some nootropic research I was conducting. I wanted to create an easy to do process that required no defat, no sodium hydroxide, had little waste. And what waste there was minimize the impact of disposing of it. This method was end product of that research. So far this method has worked without error over a number of extraction runs and I would like to share it.
I hope it helps and other people have successful results. Below is a copy and paste of my notes. It’s assumed one understands the basic use of laboratory equipment; the notes explain the process mostly and not how the equipment works.
[Acacia Confusa Alkaloid Extraction]
(No lye required)
(No defat required)
Notes:
1. This method has little hazardous waste; the hexane should be reused at the end for additional extracts from the solution and future extractions. Sodium carbonate is safe to handle and the spent plant matter can be composted as the plant matter is only subjected to water exposure. The solution its self could possibly be used as a dye once any remaining hexane evaporates and there are no toxins in the plant matter; it will stain with a dark red color.
2. In a separate experiment it was verified that the source plant matter did contain oils; by placing the plant matter in hexane for 24 hours and draining the liquid. It’s not known why this method seems to automatically remove the fat form the end product. It’s theorized that the sodium carbonate decahydrate reacts in some way with the other chemicals in the plant matter to bind the plant fats to the polar solution.
3. For step 7 further extractions should be done on the primary solution, until the solution stops yielding alkaloids. Further extractions should be done one at a time using 60ml hexane each time and allowing the 60ml to freeze precipitate before doing a another extraction.
4. Step 5 and the second part of step 7 dealing with 500ml flask are not needed if the hexane layer is siphoned off from the 1000ml flask and none of the bottom layer was picked up in the process. These steps are only done because a separatory funnel was used. The top layer can be siphoned off the 1000lm flask and placed directly into the recrystallization dish.
Material list:
50gm acacia confusa root bark (fine chips)
10gm sodium chloride
700ml water (distilled or bottled)
100gm sodium carbonate decahydrate (how to make this out of baking soda is listed at the end)
240ml hexane
1x 32oz wide mouth mason jar with vacuum seal lid
1x 1000ml Erlenmeyer flask
1x 1000ml recrystallization dish
1x 500ml Erlenmeyer flask
1x 1000ml beaker
1x 1000ml separatory funnel
2x 2" length, 3/8" diameter magnetic stir bar
1x hot plate with magnetic stirrer
1x pipette (Stepmate Repeater with 50ml Syringe Tip and a flexible tube works well)
2x Cotton Muslin Bags 5x7 Inches (bleach cleaned and allowed to dry before use) (after first use they only need to be hand washed to be reused)
1x funnel
1x coffee filter
Cling wrap
Extraction Steps:
1. Place the acacia confusa in a muslin bag folding the top over downward. Then place the first bag inside the second muslin bag. With the folded down top of the first bag against the side of the second bag. Then fold the second bag’s top over downward opposite of the first bag’s fold direction. Then Place the muslin bag combo with the acacia confusa in a mason jar so the first bag’s folded over top is facing down in the mason jar. (the folding helps keep the plant material from escaping)
2. Fill the mason jar with 700ml water. Close the mason jar with the vacuum lid. It’s important for the lid to seal tightly to retain a pressure cooking affect. Place the mason jar inside the 1000ml beaker and fill the beaker so the water line is about 1/2cm above the water line inside the mason jar. Heat water bath to 98c and allow for it to sit for 24hours.
3. Place a stir bar into the 1000ml Erlenmeyer flask. Remove the mason jar from the 1000ml beaker. Then remove the lid from the mason jar. Using the funnel pour the liquid from the mason jar into the 1000ml Erlenmeyer flask. Using gloves squeeze remaining fluid from the bag into the funnel. Place the flask on a hotplate set at 70c and begin stirring at 100 rpm. Add in 10gm sodium chloride to the solution first, and secondly add 100gm of sodium carbonate decahydrate. It should go from a dark red tea color to a black color in about 5mins. (It’s really a very dark red but it will look black)
4. After all the sodium carbonate decahydrate dissolves and the solution turns black; add in 60ml hexane using the pipet squirting the hexane on the side wall of the Erlenmeyer flask so it runs down to the solution. DO NOT shake. Turn the stirrer up to 300 rpm and keep the temperature at 70c allow it to stir for 1hour.
5. While the solution in the 1000ml Erlenmeyer flask is stir. Prepare the 500ml Erlenmeyer flask by adding 250ml water with 0.5gm of sodium carbonate decahydrate, and a stir bar to the flask.
6. After the hour as passed remove the stir bar and pour the solution from the 1000ml Erlenmeyer flask into a separatory funnel. Collect the bottom layer with the 1000ml Erlenmeyer flask. Collect the top 60ml hexane/alkaloid layer into the 500ml Erlenmeyer flask that was prepared in step 5.
7. Repeat steps 4 and 6 at least three more times. Combining the extractions into the one 500ml Erlenmeyer flask. Then place the 500ml Erlenmeyer flask on the hot plate for 15 minutes at 75c with stir set at 100 rpm. Extract the hexane/alkaloids layer, using a pipette and place it into a recrystallization dish. Cover the recrystallization dish with cling wrap and place in a chest freezer for at least 48hours.
8. After the 48 hours, using an Erlenmeyer flask with funnel and coffee filter, drain off the hexane through the filter paper to catch any floating alkaloids; allow the alkaloids in the dish and in the coffee filter to air dry in a low dust area before collection.
[How to make sodium carbonate decahydrate]
Notes:
1. This involves high temperatures and glassware wear safety gloves and eye protection.
2. It’s important that the containers are clean as a supersaturated solution will be created. Excess dust/dirt can affect the recrystallization process.
3. Store the sodium carbonate decahydrate at room temperature. Excess heat will cause it to decompose into water and sodium carbonate. A mason jar or tupperware container works well for storage.
4. The crystal clumps will be semi-opaque with some appearing in a soft white color when dry. This normal and will not affect the extraction process.
5. There is more than one way to create sodium carbonate decahydrate this method makes the crystal more “clumpy” which are quicker to dry and easier to use. Using pure water creates very thin crystals that easily decompose when touched. The thin crystals can take a week or more to dry out.
Material list:
670ml water (distilled or bottled)
200ml 190 proof ethanol (95% ethanol 5% water)
177gm sodium bicarbonate (baking soda)
1x 1000ml beaker
1x 1000ml recrystallization dish
1x fine mesh strainer
1x container the strainer can rest on top of
1x 2" length, 3/8" diameter magnetic stir bar
1x hot plate with magnetic stirrer
1x cookie sheet
1x funnel (use glass or ceramic)
Non-stick Aluminum Foil
Coffee filters
Cling wrap
Steps:
1. Place the aluminum foil over the cookie sheet. Then spread the sodium bicarbonate over the foil in a thin layer. Place in the oven at 232c for 3 hours. This will convert the sodium bicarbonate to sodium carbonate. To verify the conversion took place, the weight of the product at the end of the 3 hours it should weight about 60% less at about 106 grams.
2. Place the sodium carbonate into the 1000ml beaker add in 670ml water and 200ml ethanol. Heat the solution slowly over time until a temperature of 220c is reached. Stirring at 200rpm for 30mins.
3. After all the sodium carbonate dissolves remove the beaker from the hot plate and remove the stir bar. Using the funnel and coffee filter, filter the solution into a recrystallization dish. Cover with cling wrap. Once the solution cools to room temperature move it to the refrigerator for 24 hours.
4. After the 24 hours the sodium carbonate decahydrate should be in a semi-opaque crystals at the bottom. Setup the fine mesh strainer by resting atop a suitable container that can hold the excess water. Then slowly drain the excess water and crystals through. Allow the crystals to dry over 48-72hrs in the strainer atop the container. To verify that the crystals are sodium carbonate decahydrate they can be re-weighted, and the total should weight about 286 grams when dry.