茶からのカフェイン抽出
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液液抽出で天然アルカロイドを単離する
目的
ジクロロメタンを用いた液液抽出で茶葉からカフェインを抽出し、溶媒抽出と天然物の単離を実証する。
背景
Tea contains 2-4% caffeine by dry weight. After brewing a concentrated tea, caffeine is extracted into dichloromethane (DCM), which is immiscible with water. Sodium carbonate is added to convert tannins to sodium salts, keeping them in the aqueous layer while caffeine partitions into DCM.
安全上の警告
- DCM is a volatile organic solvent — work in fume hood
- DCM is denser than water (lower layer in separating funnel)
- Avoid inhaling DCM vapors
- Do not use open flames near DCM
必要なPPE
材料
-
Tea bags (black tea) (4 bags)Strong black tea
-
Dichloromethane (DCM) (60 mL)Extraction solvent
-
Sodium carbonate (Na₂CO₃) (5 g)To deprotonate tannins
-
Anhydrous sodium sulfate (5 g)Drying agent
-
Hot water (200 mL)Freshly boiled
器具
手順
Brew a strong tea by steeping 4 tea bags in 200 mL of hot water for 10 minutes. Squeeze out the bags and allow to cool.
Add 5 g Na₂CO₃ to the tea. Stir until dissolved.
Transfer the tea to the separating funnel. Add 20 mL DCM. Shake gently with frequent venting.
Allow the layers to separate. Drain the lower DCM layer into a clean flask.
Repeat the DCM extraction two more times with fresh 20 mL portions. Combine all DCM extracts.
Dry the combined DCM extracts over anhydrous Na₂SO₄ for 10 minutes. Filter.
Carefully evaporate the DCM in a fume hood using a warm water bath (not a hot plate directly). White caffeine crystals should remain.
Weigh the crude caffeine. Calculate the yield per gram of tea.
予想される結果
White to off-white crystalline caffeine, typically 20-50 mg from 4 tea bags. The crystals should have a bitter taste. If a melting point apparatus is available, pure caffeine melts at 235-238°C.
後片付け
Evaporate remaining DCM in fume hood before disposing of waste. Rinse glassware with acetone then water. Dispose of DCM waste in halogenated solvent container.
詳細
- カテゴリ
- Organic Synthesis
- 難易度
- Advanced (University)
- 所要時間
- 90 分
- 推定費用
- $15.00
- ステップ数
- 8
- 材料
- 5