I want to prepare ethyle acetate extraction of a fruit material for GCMS study to explore bioactive phytoconstituents. The dry and powdered fruit sample does not fully dissolve in ethyle acetate. What can i do now? can i try another solvent?
How the whole sample can be dissolved in a single solvent?
Mix your sample with the solvent of interest and then sonicate it. Compounds will get dissolve in their respective solvent and collect easily using centrifugation. The remaining pellet you can discard.
Lots of literature available to prepare extract using different solvents.
As you want to prepare an extract of Ethyl acetate that means only those phytochemicals will dissolve in Ethyl acetate which are soluble in it. Other chemicals moieties will remain insoluble in it.
Here I am sharing with you my experimental procedure for the preparation of Ethyl acetate fraction of Saraca ascoa flowers.
Saraca Asoca flowers were cleaned and shade dried at room temperature for a week. Dried flowers were subjected to particle size reduction using a mixer grinder. The coarse powder was further subjected to defatting in a Soxhlet extractor using petroleum ether at 30-40°C for about 4-5 hours. The defatted residue was dried and further extracted with methanol for about 72 hours at 60-65°C. The temperature of extraction was monitored periodically. The methanolic extract was concentrated and the yield was recorded. This extract was further dissolved in sufficient amount of methanol. This methanolic extract was mixed with equal amounts of distilled water and ethyl acetate (1:1) in a separating funnel. The funnel was shaken vigorously and the ethyl acetate layer was pulled out. The aqueous layer was washed with ethyl acetate several times. The ethyl acetate fraction thus collected was further concentrated and dried. The yield was recorded. This extract was stored under refrigeration conditions (2-8°C) until further use.
The fruit or its powder can't be fully dissolved the scattered particles will still be visible after mixing. You need to wait until the particles settles down then you can separate the ethyl extract which already have dissolved the compounds from the fruit as per its ability and then discard the crude.
You can use the rotary evap then...
What is the name of your plant? First you need to know which compounds usually contain that fruit and in relation to the components you are targeting, you choose a solvent. However, the high temperatures (300°C) used in the GC-MS injection port (and oven) can result in thermal degradation of injected molecules, thus resulting in the measurement of degradation products instead of the actual molecule(s) of interest. Because of that it is very important what kind of molecules are present in plant.
No, the plant material won't completely dissolve in any solvent. You are extracting the compounds from the solid material, and the more polar compounds aren't dissolved in the ethyl acetate.
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(PDF) Ethnicity and Scientific validation of West Bengal Amla (Phyllanthus emblica L.) with special reference to GC-MS screening (researchgate.net)
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