Paul Henry Camacho Mara Kr!ta Coo Ma# Kathleen Pearl $rande
Date Performed: February 1-4, 2016 Date "ubmtted: February 12, 2016
%&'erment 1 (!olaton of Caffene From )ea )ea Introduction
Caff Caffe ene ne or 1,*,+ 1,*,+ trm trmet ethyl hyl&an &anth thn nee th th the the chem chemcal cal formula C.H10 / /42, ! an oranc !ub!tance commonly 're!ent n coffee, tea!, enery drn! and medcne# (t ! a cry!tallne !old of hte color and btter ta!te# (t can be found n nut!, !eed and lea3e! of !ome 'lant!# (t ! dely u!ed a! a bran !tmulant due to t! effect on the central ner3ou! !y!tem hch cau!e! non-dro!ne!!, alertne!! and enery boo!t n human!# (t ! al!o con!dered a ea duretc or can cau!e lo!! of lttle amount! of flud! n the body thout dehydratn t# (t a! al!o 'ro3en that caffene can m'ro3e the metabol!m by boo!tn the metabolc rate and ncrea!e the burnn of fat!# Caffene can be addct3e too and can cau!e thdraal !ym'tom! f con!um'ton ! !to''ed after addcton# mount of caffene 're!ent n dfferent !ub!tance! can 3ary de'endn on the le3el or !nfcance of u!ae# Caffene content n ant-fatue and headache medcne ! a lot hher than tho!e n coffee and tea!# Caffene ! u!ually con!umed by human! throuh nfu!on or e&tracton n ater# ne common e&am'le of th! ! tea hch u!e! caffene-contann tea lea3e! that contan! a !mall amount of caffene of about *5# )ea ! a be3erae made by !tee'n lea3e! and leaf bud! of Camellia sinensis or the tea 'lant# )he act3e nredent! n tea are alalod rou'! th !mlar !tructure!# lalod! are m&ed m&ed rou' rou' of 'lan 'lantt con! con!t ttu tuen ent! t! that that cont conta an n a ntr ntro oen en-be -bear arn n mole molecul culee hc hch h are are 'harmacolocally act3e le theobromne and theo'hyllne# )he mo!t act3e a ct3e alalod 're!ent n tea ! caffene hch belon! to 'urne alalod rou'# (n th! e&'erment, caffene a! !olated from tea lea3e! u!n !te'-by-!te' and !'ecfc method! to elmnate other oranc com'ound! and com'onent! of the lea3e! hch ere al!o ater-!oluble le fla3onod!, cellulo!e, chloro'hyll, theobromne and other!# %&tracton a! u!ed n order to !olate the caffene from other com'ound! 're!ent n the lea3e!# "e3eral ty'e! of e&tracton a! u!ed le !oldl7ud e&tracton hch a! done n the form of bren# l!o, 87udl7ud e&tracton a! done and d!tllaton a! al!o 'erformed# l!o, certan chemcal! ere u!ed n order to elmnate other com'onent! of the tea lea3e! hch ere !'ecfc to e3ery taret com'oundcom'onent to be elmnated# )he ob9ect3e! of th! e&'erment ere to !olate the caffene form tea by e&tracton and fnd t! ma!! and 'ercent reco3ery# )he determned ma!! and 'ercent reco3ery a! com'ared to the amount clamed by the brand of tea# )he tea brand u!ed n th! e&'erment a! 8'ton )ea#
)he e&'erment a! lmted to tea lea3e! only !nce other !ub!tance! al!o ha3e a dfferent !ere! and !et! of !te'! and 'rotocol! u!ed n !e'ara tn oranc com'ound! from them Data and Results
Tea Pre-Weighed Vial Vial + Caffeine Caffeine g solute caffene 5Caffeine = × 100 g tea !am'le 5Caffeine = =
0#011: 10#0:2*
×
Weight (g) 10.0523 20.6343 20.6458 0.0115
100
0#11445
Observations
Durn the !altn out of caffene 'art, the follon ere ob!er3ed: •
fter /aCl and Ca;H<2 ere added and the !oluton a! heated for 1 mn!#, a bron, chocolate-le l7ud a! formed# )hen, after 3acuum fltraton u!n a =uchner Funnel, a dar reen to bron-colored fltrate a! athered#
)hen, durn the l7ud-l7ud e&tracton: •
fter the addton of DCM, !mall amount of ar e!ca'ed throuh the !tem of the !e'aratory funnel hen alloed to 3ent# )hen after m&n and ently !han, to layer! of l7ud ere ob!er3ed# ne th a dar bron color and lht bron color hch a! the a7ueou! layer and the oranc layer hch a! clear# l!o, bubble! ere formed at the a7ueou! layer# fter the thrd addton of DCM, more bubble! ere formed and only a !mall amount of caffene e&tract a! !e'arated and mo!t of the l7ud n the funnel a! already bubbly#
Durn d!tllaton: •
nly a !mall amount of caffene a! !e'arated and de'o!ted on the bottom of the fla!# )he !e'arated caffene e&tract had an aromatc and fre!h tea drn-le !mell#
8a!tly, durn dryn: "mall amount of hte cry!tal! ere de'o!ted at the !de and bottom of the 3al# )he cry!tal! !tll al!o had an aromatc !mell#
Discussion
(n th! e&'erment, one of the man ob9ect3e! ! to !olate the caffene from tea throuh method! of e&tracton and d!tllaton# (n the e&tracton 'roce!!, caffene a! !olated throuh !altn out th ater# (n th! 'roce!!, after addn 100m8 of boln ater to the 're-ehed tea ba! and 're!!n out a! much ater, !odum chlorde and calcum hydro&de ere added to the e&tracted !oluton# "odum chlorde a! added becau!e ater ll be attracted to !alt hch ll lea3e the le!! 'olar caffene, thu!, !olatn t# >1? l!o, calcum hydro&de a! added to react th the tannn! 're!ent n tea to !olate the!e com'onent! from caffene# ddn calcum hydro&de al!o mae! the !oluton ba!c# @nd!!ol3ed !old! ere !e'arated u!n a =uchner funnel# >1? nother 'rocedure done n th! e&'erment a! the l7ud-l7ud e&tracton of caffene# (n th! 'roce!!, dchloromethane ;DCM< a! added to the tea e&tract# )h! a! done to d!!ol3e the tea !nce t ! more !oluble n DCM than n ater# fter the addton of DCM, the !oluton a! m&ed by ently rocn t to a3od formaton of emul!on!# Durn the e&'erment, !alt a! added e3ery tme there ! 're!ence of AntolerableB amount! of emul!on!# )he oranc layer a! then draned !e'aratn t from the a7ueou! layer# )h! hole 'roce!! a! re'eated three tme!# )he thrd 'art of the 'rocedure a! the a!hn and dryn of caffene e&tract# )he caffene e&tract a! a!hed th 105 !odum hydro&de !oluton# )h! a! done to mnme caffene lo!t alon the 'roce!!# )he e&tract !oluton a! tran!ferred nto an %rlenmeyer fla! and a! dred by addn anhydrou! !odum !ulfate# )here a! a formaton of !lhtly !old com'ound hch a! decanted and u!ed for the d!tllaton 'roce!!# (n the d!tllaton 'roce!!, the e&tracton !ol3ent a! d!tlled from the caffene e&tract u!n a ater bath a! a heat !ource# )he tem'erature a! montored untl t reached 40 deree! Cel!u!, 9u!t n tme hen the fla! ! dry and no more d!tllate ! ben collected# )he crude caffene re!due a! tran!ferred nto a 're-ehed 3al, rn!ed th !mall amount! of acetone and a! e&'o!ed to ar to e3a'orate the acetone# )he 3al a! ehed aan to determne the ma!! of caffene# (n th! e&'erment, the 'o!!ble !ource! of error ere the 1< 're!ence of ntolerable amount! of emul!on durn the l7ud-l7ud e&tracton, 2< contamnaton of e&tract! and !oluton! alon the 'roce!! !nce th! a! a lenthy e&'erment and *< m'urte! that mht be 're!ent n the contaner! and la!!are! u!ed n the e&'erment#
Conclusion and Recommendations Extraction is a method for the separation of organic compound from a mixture. In this experiment caeine was extracted from tea. Dierent processes were undergone in order to isolate caeine from tea. Caeine was rst salted out by adding NaCl and Ca!"#$% li&uid'li&uid extraction followed% by adding dichloromethane to separate the organic compound. It was then washed and dried ready for distillation. Crude caeine was the resulting residue. (he mass of the crude caeine was ).)**+g and the computed percent caeine is ).**,,-. (he claimed mass caeine of ipton /ellow (ea is ).))++g per bag. In the experiment where approximately 0 bags were used% the calculated gram caeine reco1ered was ).)**+g. (he reco1ery of the caeine was 1ery small due to some errors made during the experiment. 2ome reactions may ha1e not gone into completion or there was a loss of sample during transfer or during some certain procedures.
(o impro1e the reliability of the results of the experiment% it is recommended that the experiment be conducted in * meeting to a1oid contamination of extracts and solutions along the process. 3lso% it recommended that the glasswares and apparatuses used be properly washed and free from impurities that might cause error. 4uestions and 3nswers5 Discuss the role6s of the following in the isolation of caeine5 1 a Dichloromethane' (his is an organic sol1ent used in li&uid'li&uid extraction because caeine is more soluble in dichloromethane than in water.7*8 b Na!" a&ueous solution' 2odium "ydroxide is a basic solution% it is used to remo1e impurities and minimi9es the caeine lost. 7*8 c Ca!"#$ ' 2ince Calcium hydroxide is a base and tea is consist of other components including chlorophyll% tannins and :a1onoids which are acidic% Ca!"#$ will react with tannins to form salt. (his will isolate them from caeine. (his also ma;es the solution basic. 7*8 Explain why salt was added to the water before the li&uid'li&uid extraction of caeine. cient is the extraction of tea lea1es containing *.)g of caeine with ? $)'m portions of dichloromethane o1er that of a single step extraction= It is e>cient to extract caeine from tea with ? $)m portions of dichloromethane o1er that of a single step extraction for it can obtain much of the pure sample. It extracts the caeine that where not extracted from the pre1ious one. 7*8
Retrie1ed Arom Retrie1ed
7?8 B9unalic% 3mra% et. al.% Extraction of acti1e ingredients from green tea Camellia sinensis#5 Extraction e>ciency of maor catechins and caeine. Else1ier. une $))0. Retrie1ed from http566www.sciencedirect.com6science6article6pii62)?)*,0)+))$0*F. Retrie1ed Aebruary *% $)*0. 7,8 Caeine. Drugs.com. Retrie1ed Aebruary *% $)*0.
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from
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7+8 Caeine Content for Coee% (ea% 2oda and more. Nutrition and healthy eating. @ayo Clinic. Retrie1ed from http566www.mayoclinic.org6healthy'lifestyle6nutrition' and'healthy'eating6in'depth6caeine6art'$)),G?H$. Retrie1ed Aebruary *$% $)*0. 708 ersad% eeana% Energy drin;s and the neurophysiological impact of caeine. Arontiers 3rchi1e. Retrie1ed from http566ournal.frontiersin.org6article6*).??G6fnins.$)**.))**06full. Retrie1ed Aebruary *% $)*0.
