TRNG I HC CNG NGHIP TP.

H CH MINH KHOA CNG NGH HA HC

N CHUYN NGNH

THIT K H THNG CHIT LNG LNG V CHNG CT BN T NG

GVHD: Th.s TRN NGUYN AN SA Lp: CDPT12 Kho: 2010 - 2013

Tp. H Ch Minh, thng 04 nm 2013

CHNG 1: TNG QUAN L THUYT

1.1. Tng quan v chng ct

1.1.1. Nguyn tc chung ca chng ct Chng ct l mt k thut tch v tinh ch cc cht da theo im si (nhit si) ca chng tch cc cht theo tng phn on khi chng ct trong nhng iu kin nht nh. Vic chng ct c th ly c ring tng cht hay mt nhm cht ty thuc vo trang thit b v iu kin (nhit ) c khng ch khi thc hin chng ct. 1.1.2. Cc k thut chng ct 1.1.2.1. Chng ct thng thng y l qu trnh chng ct tinh ch cc cht ch da theo im si ca chng tch cc cht theo tng phn on trong nhng iu kin bnh thng theo nhit v s bay hi khi chng ct. ngha l trong iu kin bnh thng mi cht c nhit si v c p sut khc nhau. V th khi chng ct mi cht s c ngng t ti mt phn on khc nhau. 1.1.2.2. Chng ct li cun hi nc y l qu trnh chng ct tinh ch v tch cc cht cng da theo im si ca chng tch cc cht theo tng phn on trong nhng iu kin nht nh theo nhit si v bay hi khi chng ct, nhng trong trng hp ny, cht phn tch cn chng ct khng bay hi mt mnh tt, m phi c mt cht khc c nhit si gn hay bng n li cun n i theo th mi chng ct n c tt. V th gi l chng ct li cun. Lc ny thu c sn phm l dung dch ca cht li cun. 1.1.2.3. Chng ct p sut thp (ct quay chn khng) y l qu trnh chng ct tinh ch cc cht cng da theo im si ca chng tch cc cht theo tng phn on trong nhng iu kin nht nh theo

nhit v s bay hi ca cht phn tch. Khi chng ct trong mi trng p sut thp Ngha l trong iu kin ny, mi cht cng c nhit si v bay hi khc nhau, khc iu kin bnh thng. V th khi chng ct mi cht s c thu li theo mt phn on khc nhau. Cch chng ct ny thng l giai on th hai, lm bay hi dung mi chit ca qu trnh x l mu chuyn mu ha tan trong dung mi khc th mi xc nh c n.

1.2. Tng quan v chit lng - lng

1.2.1. Nguyn tc Nguyn tc ca k thut chit ny l hai pha lng (dung mi) khng trn ln c vo nhau (trong hai dung mi ny, c th c mt dung mi c cha cht phn tch c trong mt dng c chit nh phu chit, bnh chit). Khi lc chit cht phn tch s c phn b vo hai dung mi theo tnh cht ca chng, t n trng thi cn bng. V th h s phn b nhit ng Kb ca cn bng chit l yu t quyt nh hiu qu ca s chit. 1.2.2. iu kin chit c c kt qu chit tt, qu trnh chit phi c cc iu kin v m bo c cc yu cu nht nh sau y: Dung mi chit phi tinh khit cao, khng lm nhim bn thm cc cht phn tch vo mu. Dung mi chit phi ha tan tt cc cht phn tch, nhng li khng tt vi cc cht khc c trong mu. H s phn b ca h chit phi ln, cho s chit c trit . Cn bng chit nhanh t c v thun nghch, gii chit c tt. S phn lp khi chit phi r rng, nhanh v d tch ra ring bit. Phi chn pH, hay mi trng acid, loi dung mi thch hp. Chn nhit ph hp v phi gi n nh sut qu trnh. Phi thc hin lc mnh u trong qu trnh chit. Cho thm cht chng to khi cn c s phn lp tt.

1.2.3. Cc phng php chit lng lng 1.2.3.1. Phng php chit tnh Phng php chit ny rt n gin, khng cn my mc phc tp, m ch cn mt s phu chit (dung tch 100, 250, 500 mL) l c th tin hnh c mi phng th nghim. Vic lc chit c th c thc hin bng tay, hay bng my lc chit nh. Tt nhin kh lm hang lot mu th mt nhiu thi gian. 1.2.3.2. Phng php chit dng chy lin tc Trong phng php chit ny, khi thc hin chit, hai pha lng khng trn c vo nhau (hai dung mi, c mt dung mi c cha cht phn tch) c bm lin tc vi tc nht nh qua h chit nh phu chit hay bnh chit lin hon ng kn. Hoc cng ch c th ch mt dung mi chuyn ng, cn mt pha ng yn. Khi cht phn tch s c phn b vo hai dung mi theo tnh cht ca chng, t trng thi cn bng. V th y h s nhit ng K l yu t quyt nh hiu qu ca s chit. Chit theo cch ny nhanh, hiu qu cao. y l phng php chit c ng dng nhiu trong chit sn xut cng ngh. 1.2.3.3. u nhc im v phm vi ng dng Phng php chit tnh n gin d thc hin, c ng dng ph bin v rt c hiu qu trong lnh vc tch chit phn tch, v lm giu cc cht phn tch phc v cho vic xc nh hm lng vt ca chng trong mu. Nht l tch v lm giu cc kim loi, cc cht hu c c hi trong cc loi mu nc, nc thi, nc bin, nc khong. Cc u v nhc im chung ca k thut chit l: Thch hp cho c chit phn tch v sn xut tch chit lng ln. Loi c cc nh hng, nht l cht nn ca mu. Thch hp cho lm giu lng nh cht phn tch. Phc v cho chit c c cc cht mu v c v hu c.

1.3. Tng quan v hp ph

1.3.1. nh ngha hp ph

Hp ph l qu trnh t tp (cht cha, thu ht) cc phn t kh, hi hoc cc phn t, ion ca cht tan ln b mt phn chia pha. B mt phn chia pha c th l lng - rn, kh - lng, kh - rn. Cht m trn b mt ca n c s hp ph xy ra gi l cht hp ph, cn cht m c t tp trn b mt phn chia pha c gi l cht b hp ph. B mt tnh i vi mt gam vt mt gam vt hp ph gi l b mt ring ca n. Nhng vt khng c l xp c b mt ring t vi m 2/gam n vi tram m2/gam. Qu trnh hp ph l qu trnh ta nhit, hiu ng nhit ca qu trnh hp ph c gi l nhit hp ph. 1.3.2. Phn loi 1.3.2.1. Hp ph vt l Hp ph vt l: Cc nguyn t b hp ph lin kt vi nhng tiu phn (nguyn t, phn t, cc ion) b mt phn chia pha bi lc lin kt Vander Waals yu. Ni mt cch khc, trong hp ph vt l cc phn t ca cht b hp ph v cht hp ph khng to thnh hp cht ha hc (khng hnh thnh cc lin kt ha hc) m ch b ngng t trn b mt phn chia pha v b gi li trn b mt bng lc lin kt phn t yu (lc Vander Waals) v lin kt hidro. S hp ph vt l lun lun thun nghch, nhit hp ph khng ln. 1.3.2.2. Hp ph ha hc Hp ph ha hc: c nhng lc ha tr mnh (do cc lin kt bn ca lin kt ion, lin kt cng ha tr, lin kt phi tr) lin kt nhng phn t hp ph v nhng phn t b hp ph to thnh nhng hp cht ha hc trn b mt phn chia pha. Ni mt cch khc hp ph ha hc xy ra khi cc phn t hp ph to hp cht ha hc vi cc phn t b hp ph v hnh thnh trn b mt phn chia pha (b mt pha hp ph). Lc hp ph ha hc khi l lc lin kt ha hc thng thng

(lin kt ion, lin kt cng ha tr, lin kt phi tr) s hp ph ha hc lun lun bt thun nghch. Nhit hp ph ha hc ln, c th t ti gi tr 800kJ/mol.

1.4. Tng quan v du m v cc ch tiu nh gi du m

1.4.1. Khi qut chung v lipid Lipid l thnh phn c bn ca vi sinh vt, ng vt v thc vt. Lipid l mt trong thnh phn quan trng ca ba n v chng c nng lng cao nht so vi glucid v protid (1g lipid cung cp 9.3 Kcal, trong khi 1g glucid cung cp 4.1 Kcal v 1g protid cung cp 4.2 Kcal); cha nhiu loi acid bo khng bo ha rt cn thit m c th khng t tng hp c. V cu to ha hc, hu ht cc loi lipid u c acid bo v ancol. Trong thnh phn cu to lipid, khng c hoc c rt t cc nhm u nc nh OH, -NH 2, -COOH v c rt nhiu nhm k nc. Chnh v vy lipid khng hoc rt t ha tan trong nc m ha tan nhiu trong dung mi c phn cc thp nh cc dung mi hu c (ether, benzene, chloroform). V vai tr cu to, lp m di da v lp m bao quanh mt s c quan c tc dng bo v cho c th v cc c quan. Cc phc hp ca lipid vi protein gi l lipoprotein l nhng thnh phn cu to quan trng ca t bo, thng thy c mng t bo v trong ty th. Cc lipoprotein cn ng vai tr vn chuyn trong mu. Trong ngn ng thng thng, lipid cn c gi l cht bo v bao gm cc cht du, m, sp. nhit thng, m v sp thng th c, du th lng. Lipid gm nhiu loi khc nhau v c th sp xp theo nhiu cch. C th phn loi nh sau: lipid n gin v lipid phc tp. 1.4.2. Thnh phn cu to ca lipid Lipid l nhng sn phm ngng t ca cc acid bo v ancol. Cng c th nh ngha lipid l nhng este hoc amin ca acid bo v ancol hoc amin ancol. 1.4.2.1. Acid bo a. Acid bo bo ha

Acid bo bo ha c cng thc tng qut l C nH2n+1COOH, acid acetic c coi nh cht u tin trong cc loi acid. Bng 1.1. Mt s acid bo bo ha c trong thin nhin. Tn acid Acetic Butyric Caproic Lauric Myristic Palmitic Stearic Arachidic Lignoceric Cng thc CH3COOH CH3(CH2)2COOH CH3(CH2)4COOH CH3(CH2)10COOH CH3(CH2)12COOH CH3(CH2)14OOH CH3(CH2)16COOH CH3(CH2)18OOH CH3(CH2)22COOH Tn h thng Acid n-etanoic Acid nbutanoic Acidnhexanoic Acid ndodecanoic Acid ntetradeecanoic Acidnhexadecanoic Acid noctadecanoic Acid neicosanoic Acid tertracosanoic B ca b, d nng chy (0C) C trong thin nhin

Du da

M ng thc vt

Du lc, sp ng thc vt

Ngoi cc acid bo trn cn gp nhiu acid bo bo ha bc cao hn, nht l trong cc cht sp. Ngi ta cn thy mt s acid bo bo ha c nhnh t ngun gc cy c v ng vt. b. Acid bo khng bo ha L nhng acid bo chui thng (i khi c nhnh), chia thnh nhiu loi ty theo mc khng bo ha. b.1. Loi c mt lin kt i (acid bo polyethylenic)

CTTQ: CnH2n-1COOH. Acid bo oleic l mt acid bo khng bo ha rt ph bin, c trong tt c cc du m ng vt, thc vt nh: Trong m d tr ca b v ln (40%), du olive (80%). b.2. Loi c nhiu lin kt i Loi c hai lin kt i: CTTQ: CnH2n-3COOH, nh acid linoleic c trong nhiu loi ht c du. Loi c ba lin kt i: CTTQ: CnH2n-5COOH, thng c cng vi acid linoleic, nhng c bit c trong du lanh. Loi c bn lin kt i: CTTQ: C nH2n-1COOH, nh acid arachidonic ch yu trong du lc. c. Acid bo mang cha ancol Acid cerebronic c trong lipid tp no: Bng 1.2. Mt s acid bo khng no thng gp Tn acid Acid palamiolei c Acid oleic Acid linoleic Acid linolenic Acid arachidoni c d. Cng thc cu to im nng chy - 0,5 13,4 5 -11

CH3(CH)5CH=CH(CH2)7COOH CH3(CH2)7CH=CH(CH2)7COOH CH3(CH2)4CH=CHCH2CH=CH(CH2)7COOH CH3CH2CH=CHCH2CH=CHCH2CH=CH(CH2)7COOH CH3(CH2)4CH=CHCH2CH=CHCH2CH=CHCH2CH=C H(CH2)3COOH

-49,5

Acid bo c vng

Acid prostanoic l mt acid c vng 5 cnh vi 20 carbon v mang 2 chui thng. Acid prostanoic c dn xut l prostaglandin.

e.

S ng phn ca acid bo khng bo ha Cc acid bo khng bo ha tn ti di nhiu dng ng phn l do v tr ca

cc lin kt i trong chui carbon ca acid bo to ra. Acid oleic c th c ti 15 dng ng phn v tr khc nhau. ng phn hnh hc ca ancol bo khng bo ha l do phng hng ca cc gc xung quanh trc ca lin kt i to ra. Mt s cht ch khc nhau v phng hng ca cc phn xung quanh trc ny. Nu nhng gc ang c xem xt v cng mt pha ca lin kt i th hp cht c gi l dng cis, nu gc nhng hng tri ngc nhau th hp cht c gi l dng trans. Vi nhng acid bo c khng bo ha ln hn, ngha l c nhiu lin kt i hn th c ng phn hnh hc hn. Nhng acid bo khng bo ha chui di, thng gp trong t nhin th hu nh u thuc dng cis v phn t b un cong v tr lin kt i. f. Tnh cht ha hc ca acid bo

f.1. Tnh cht ha hc do nhm carboxyl S to thnh mui: acid bo tc dng vi cc hydroxyl kim loi (NaOH hoc KOH) to thnh mui kim ca acid bo tc x phng. X phng tan trong nc v c tnh cht to bt. Nhng mui ca acid bo vi kim loi nng nh mui Ca, Mg, Zn ca acid bo u khng tan trong nc. Ngi ta ng dng tnh cht ny o cng ca nc.

S to thnh este: iu ch este methylic bng cch tc dng giu acid bo vi methanol cng s c mt ca cht xc tc.

f.2. Tnh cht ha hc do s c mt lin kt i Phn ng cng: acid bo khng bo ha tc dng vi halogen (brom hay iod) to ra cc dn xut cha halogen ca acid bo. Phn ng ny ng dng trong vic xc nh ch s iod ca acid bo (tc lng iod gn vo 100g acid bo). Ch s iod cng cao th s lien kt i trong phn t acid bo cng nhiu. Phn ng kh: Vi s c mt ca cht xc tc, acid bo khng bo ha c kh tr thnh andehyd. Cc cht chng oxy ha (antioxidant) c th ngn nga s t oxy ha ny ca acid bo khng bo ha. 1.4.2.2. Ancol ca lipid 1.4.2.2.1. Glycerol Glycerol l mt a ancol (c ba chc ru), tham gia trong thnh phn ca glycerid v phosphatide. V tr cc nguyn t carbon trong glycerol c ghi bng ch s 1, 2, 3 hoc k hiu . C th xc nh s c mt ca glycerol bng phn ng to acrolein khi un nng glycerol trong mi trng c KHSO4. 1.4.2.2.2. Cc ancol cao phn t Nhng ancol ny thng tham gia trong thnh phn cc cht sp, v d: ancol cetylic C16H36OH, ancol n- hexacosanol: CH3(CH2)24CH2OH, ancol n- octacosanol: CH3(CH2)26CH2OH, ancol n- triacontanol: CH3(CH2)28CH2OH. 1.4.2.2.3. Aminoancol Cc aminoancol tham gia trong thnh phn ca cerebrosid v mt s phosphatid. Cc aminoancol thng gp l sphingosin, colaamin (ethanolamine), choline (colamintrimethylamin), serin, cerebrin (c trong nm men, ht ng).

1.4.2.2.4. Sterol L mt nhm nhng cht c nhn cyclopentanoperhydro phenantren gm ba vng 6 cacbon: A, B, C v mt vng 5 cacbon: D, c hai nhm methyl v tr C 10 v C13, c mt hay nhiu chc ancol (- OH) m khng c nhm cacbon (CO) hoc nhm cacbon (COOH), c mt mch nhnh tt 8 n 10 nguyn t cacbon v tr C17. Cht tiu biu cho cc sterol m ng vt l cholesterol. Cht ny c trong hu khp cc t bo ca c th, c bit l trong cc m thn kinh, trong mt v si mt, vt vng ca bung trng. Cht ny c trong cht bo ng vt nhng khng c trong cht bo thc vt. Trong cc m v cc dch c th ng vt, cholesterol di dng t do hoc dng este ha vi acid bo gi l cholesterid. Cholesterol kt tinh di dng vy ng nh nh x c, ha tan trong ete v hiu dung mi hu c khc. V cu to ha hc, cholesterol l hp cht c cha chc ancol (-OH) v tr C3, c lin kt i gia C 5 v C6, c mch nhnh l nhm methyl C 10 v C13, mch nhnh gm 8 cacbon v tr C 17. Trong t nhin, ngi ta cn gp cc loi sterol khc nh 7 dehydrocholesterol, ergosterol 1.4.3. Phn loi lipid 1.4.3.1. Lipid n gin 1.4.3.1.1. Glycerid (Acylglycerol) Glycerid c trong hu ht t chc ca tt c sinh vt, nhng c bit c nhiu nht t chc m (90%). Glycerid do cc ngun gc ng vt v thc vt khc nhau v thnh phn cu to acid bo. ng vt, glyceid tp trung nhiu lp m di da v bao quanh mt s c quan bo v cho c th v cc c quan khi b lnh v b chn ng. Glycerid cung cp nhiu nng lng, 1g glycerid cho khong 9 Kcal. a. Cu to ha hc ca glycerid

Glycerid l este ca glycerol v acid bo, l cht bo trung tnh. Glycerol c ba chc ru, do vy ty theo mt, hai hay ba chc ru ca glyceol c este ha bi acid1 bo m to nn monoglycerid, diglycerid v triglycerid. Cc acid bo trong mt phn t glycerid c th ging nhau nhng c th khc nhau (glycerid thun nht v glycerid khng thun nht hay glycerid hn hp). cc phn t triglyceride c cha cng mt loi acid bo thng chim mt t l nh. Ty theo thnh phn cu to ca acid bo m glycerid c tn gi khc nhau. Nh tristearin l triglyceride c ba gc acid bo u l acid stesric, tripalmitin l triglyceride c ba gc acid bo l acid palmitic, 1.2 distearopalmitin l triglyceride c hai gc acid stearic v tr C1 v C2 v mt gc acid palmitic. Trong t nhin, diglycerid v monoglycerid thng ch chim mt t l rt nh. Do thnh phn acid bo v v tr ca cc gc acid bo trong phn t, m cc glycerid thng tn ti di nhiu dng ng phn, ch nhng triglyceride m cc gc acid bo u thuc cng mt loi l khng c ng phn, nhng triglyceride c c acid bo v tr C1 v C3 khng ging nhau th C2 l cacbon bt i v khi c th c hai dng ng phn I v II, phn ln triglyceride thin nhin dng ng phn II. b. Tnh cht l ha ca glycerid Tnh cht l ha ca glycerid ch yu l do thnh phn ca acid bo quyt nh. Glycerid cha nhiu acid bo no thng th c v gi l m, glycerid cha nhiu acid1 bo khng no thng th lng v gi l du. Hm lng acid bo mch ngn v acid bo khng no cng ln th nhit nng chy ca glycerid cng thp. c. Tnh cht ha hc ca glycerid V khng tan trong nc nn glycerid rt kh thy phn. Tuy nhin, c th thy phn glycerid bng kim, bng acid hoc enzyme lipase, kt qu l ln lt cc lien kt este dc ct dt v to thnh diglycerid, monoglycerid, glycerol v acid

bo. S thy phn cht bo bng kim dc gi l x phng ha, sn phm glycerol v mui ca acid bo gi l x phng. X phng l nhng cht ty ra nh tc dng chuyn thnh nh tng. Mt s x phng c trng lng phn t cao v c khng bo ha ln l nhng cht st khun. mt s x phng khc c tc dng kh c, chng c t bch hu v un vn. Tnh cht ca cc cht bo c c trng bi cc ch s sau: Ch s x phng ha: l s milligram KOH cn thit x phng ha 1gram du hay m. Ch s ny t l nghch vi trng lng phn t ca du, m. Ch s acid: l s milligram KOH cn thit trung ha acid bo t do ca 1 gram m. Ch s ny gip cho vic tm hiu lng acid bo t do ca du, m. Ch s iod: l ch s th hin mc khng no ca acid bo khng no trong du, m. cc cht du c ch s iod cao hn so vi cc cht m v du c nhiu acid bo khng no hn m. Mt c im cn lu l sau mt thi gian, cc cht bo thng b i, c mi v kht kh chu. l do cc lin kt i ca acid bo khng no trong phn t cht bo c th b oxi ha to nn nhng lin kt peroxyd, ri to thnh nhng andehyd v acid bo bay hi. 1.4.3.1.2. Sterid Sterid l este ca acid bo vi ancol vng l sterol (tiu biu l cholesterol). Mt s sterid l oleatcholesterol, palmitacholesterol. 1.4.3.1.3. Cerid Cerid l este ca acid bo chui di vi ancol c trng lng phn t cao ( t 30 n 40 cacbon). Cerid hay cn gi l sp, sp c trong ng vt cng nh thc vt. Sp ng vt hay gp l sp ong, m c (m cu ng vt d tr di nc). thc vt, sp to thnh mt lp mng bao ph ly l, thn v qu. V vi khun Kock v mt s vi khun khc c cha sp.

Chng nhn sinh hc ca cerid khc nhau ty loi nhng ni chung cerid gi vai tr bo v cc t chc ng vt cao cp v ngi khng chuyn ha c cerid. Sp c dng rng ri d lm nn, sp bi v cc thuc cao. 1.4.3.2. Lipid phc tp 1.4.3.2.1. Photpholipid Photpholipid l nhng este ca cc ru a chc vi cc acid bo cao v c gc acid photphoric v nhng baz cha nit ng vai tr l cc nhm ph b sung.Trong thnh phn ca cc photpholipid khc nhau, ngi ta tm c 3 trong s cc ru a nguyn t: glixerin, inozit, sphingzin:

Mezoinozit CH2OH CHOH CH2OH

Sphingozin (trans 3,1 dioxy 2 amin octa dexen 4) Do cc photpho lipid c chia thnh 3 nhm: glixerophospholipid, inozitphospholipid v shingophospholipid. Glixerophospholipid thng c gi l phosphatit, v chng c th xem l cc dn xut acid photphatric.

Acid photphatidic Trong cc phn t ca photpholipid thng c acid palmitic, acid stearic, acid linoleic, acid arachidonic cng nh acid lignoxeric, acid nervonic,

Thnh phn ca photpholipid thng c mt phn t acid photphoric, mt vi loi inozitpotpholipid c hai gc acid photpholipid. Cc baz nit ca photpholipidrat6 khc nhau v thng gp l nhng dn xut ca etanolamin. l colin v serin.

Etanolamin

Acid amino - oxypropionic

Hydroxyl ca trimetyloxyetylamin Cu to ha hc ca phospholipid ta thy rng trong phn t ca dung mi. Gc hydrocacbon ca cc acid1 bo cao to thnh vng k nc, cn cc gc ca acid phospholipid v cu baz nit vn c kh nng ion ha th to thnh vng u nc. nh c tnh m phospholipid tham gia vo vic m bo tnh thm mt chiu ca cc mng cu trc di t bo. Khi hng vng k nc v pha mi trng ngoi, cc phospholipid c th xc tip vic hp th cc hp cht khng phn cc ha tan trong cht bo (tng tc cc gc hydrocacbon) t mi trng ngoi v chuyn chng vo trong cu trc di t bo. Cc phosphor c gc colin, c lin quan vi vai tr, chc nng ca chng trong c th. Colin c axetyl ha, tc l axetylcolin rt hot ng v mt sinh l v c mt ngha ln i vi hot ng ca m thn kinh l cht chuyn s kch thch thn kinh.

Etanolamin

Acid amino - oxypropionic

Axetylcolin

Phospholipid l nhng cht rn, v sc nhng ha thnh mu ti sm rt nhanh ngoi khng kh do s oxi ha cc lin kt i ca cc acid bo cha no c trong thnh phn ca chng. Chng ha tan rt d trong benzene, trong ete du ha, trong chloroform, v.vchng khng tan trong nc, nhng c th to thnh cc huyn ph phosphate kh bn v trong mt s trng hp chng to thnh cc dung dch keo. Trong cc ht thc vt, trong tim gan ca ng vt, trong trng ca gia cm, c rt nhiu phospholipid. Phospholipid rt d to thnh phc hp vi protein dng phospholipoproteit. Chng c mt trong tt c cc t bo ca ngi, ng vt, thc vt v vi sinh vt, vi t cch tham gia ch yu trong vic hnh thnh nn v t bo v cc mng ni t bo. a. Glixerophospholipid Glixerophospholipid hay l phosphatit l nhng este ca glixerin vi acid bo cao v vi acid phosphoric c nh baz nit. Cng thc tng qut ca phosphatit c trnh by sau:

glixerophotphatit y R1 va R2 la cac gc hydrocacbon cua acid beo cao con X la baz nit. Cac hp cht loai nay u la nhng glixerophosphat, vi gc acid phosphoric lin kt vi nguyn t cacbon cung cua glixerin. Hinh nh trong thin nhin glixerophosphatit khng co

glixerophotphatit Tuy theo c tinh cua baz nit ma ngi ta chia ra cac phosphatit ra thanh colin phosphatit (lexitin), colaminphosphatit (xephalin), serinphosphatit va treoninphosphatit:

Lexitin xephalin Hinh nh lexitin, xephantin va serinphosphatit co th bin i ln cho nhau vi chung chi khac nhau bi cu tao cua cac baz. Gia cac cht nay vi du co th co s lin quan di truyn nh sau:
Kh cacboxyl

colin Vic bin i tng h cua cac phosphatit khac nhau ro rang co th tin hanh khng nhng chi do s cai bin cua cac baz nit ma con bng cach thay th hoan toan bi cac baz nay. Vi co cu to bin i (nguyn t cacbon th hai cua gc glixerin lun lun bt i) cho nn phosphatit co tinh hoat quang va tao thanh cac ng phn lp th tng ng.

Etanolamin

Acid amino - oxypropionic Axetylcolin

colin

Khi thuy phn bng kim nhe thi chi lin kt este gia acid beo va glixerin bi t, chng han khi thuy phn bng kim nhe phosphatitdylcolin se c san phm la glixerol-3-phosphary. Hp cht ny s b phn gii khi thy phn bng acid. Photphatit cng c th b thy phn bng nhng enzim c hiu gi l photpholipaza. Photpholipaza thng c chia ra nhng enzim sau: Photpholipaza A c trong nc rn ch tch c gc acid bo v tr . Do sn phm to thnh c tn gi lizophotphatit. Trong t bo v m bnh thng khng c lizophotphatit. Lizophotphatit ph hy mng nn c. Photphalipaza B tch c gc acid bo th hai (hoc c hai gc). Khi x l photphatidylcoin bng photphalipaza B ta s thu c glixerol 3 photphorylcolin. b. Photpholipaza C th xc tc thy phn lin kt gia acid photphoric va glyxerin. Cn photpholipaza D th tch c gc baz hu c. Inozitphotpholipid Cu to ca nhm photpholipid ny vn cha r. Ngoi inozit (1 mol), acid photphoric (1 2 mol) v acid bo cao (1 2 mol) khi thy phn cc inozit photpholipid cn thy glixerin (1 mol), galactoza v acid tartric. Khi c mt hai gc acid photphoric trong phn t in-ozitphotpholipid th hai nhm photphat s lin kt vi gc inozit v tr mta: V cng thc ca diphotphoinozit c th trnh by nh sau:

Inozitol_M_diphotphat

Nu cho rng inozit c rt nhiu ng phn khng gian do s phn b khc nhau ca cc nguyn t hydro v ca cc nhm hydroxyl so vi mt phng ca vng th niozit photpholipid c rt nhiu dng ng phn. Cng cn ni thm rng t u tng v t m no, ngi ta chit xut c mt inozitphotpholipid rt phc tp, c tn l lipozol. Khi thy phn hon ton lipozol s c inozit, acid photphoric, acid tartronic, galactoza, etanolamin v cc acid bo. Lipozol c cng thc nh sau: c. Sphingolipid Sphingolipid hoc sphingomielin cng u l nhng este c to nn t acid bo, colin, acid photphoric v amin ru cha no gi l sphingozin

Sphingozin Khc vi cc photpholipid khc xt trn, gc acid bo cao trn phn t sphingolipid c kt hp vi amin ru hai nguyn t bng lin kt peptit (ngha l acid bo khng phi c kt hp vi nhm hydroxyl ca ru m kt hp vi nhm amin ca amin ru):

Cc phn t khc cn li ca sphingolipid tc l acid photpholipid tc l acid photphoric v colin u c kt hp nh photphatit. Chnh trong sphingolipid ngi ta pht hin c acid lignoxeric v acid nervonic vi mt lng ng k, cc loi acid bo ny c t hn trong cc photpholipid khc.

Cc sphingolipid c trng i vi th gii ng vt hn so vi th gii thc vt. Tuy nhin t cc photpholipid c ngun gc thc vt (t ht ng) ngi ta tch c amin-ru hon ton ging sphingozin gi l phitosphingozin v c cng thc nh sau:

Phitosphingozin Sphingozin khng ha tan trong ete etylic. Tnh cht ny c dng chit xut chng ra khi cc photpholipid khc. Cu hnh khng gian rt phc tp vn lin quan ti hin tng ng phn quang hc (hai nguyn t cacbon bt i trong phn t) v lin quan ti hin tng ng phn cis trans v tr lin kt i l c tnh quan trng ca cc sphingolipid. Tnh c hiu v loi v tnh c hiu ca cc c quan u c lin quan n vn ny. 1.4.3.2.2. Glicolipid Glicolipid l nhng lipid phc tp khng c photpho. Chng c c trng ch l trong thnh phn ca chng c cu t gluxit, thng l galactoza hoc l cc dn xut ca galactoza (N axetylgalactozamin, lactoza, ). Ngi ta chia glicolipid ra lm hai nhm l xerebrozit v gangliozit. a. Xerebrozit Xerebrozit c to nn t amin ru hai nguyn t cha no sphingozin, acid bo v galactoza. Cc xerebrozit ring bit khc nhau bi cc acid bo c trong thnh phn ca chng. Nhng acid bo ny u c to nn t 24 nguyn t cacbon v c th c lin kt i v cc nhm hydroxyl. Cu to ca xerebrozit c th trnh by di dng cng thc chung sau y:

 y R1 trong cc xerebrozit l OH, cn trong sulfatit R1 l SO3H, R2 l gc acid bo (acid stearic, acid lignoxeric, acid nervonic, acid xerebronic, vv.), acid bo ny c kt hp vo sphingozit nh lin kt peptit CO NH . Cc cht in hnh ca xerebrozit l xerebron (hoc frenozin), kerazin, nervon, oxynervon. Trong phn t xerebron c acid xerebron CH 3 (CH2)12 CHOH COOH, trong phn t kerazin c acid lingoxeric CH 3 (CH2)13 COOH, trong phn t nervon c acid nervonic cha no CH 3 (CH2)7 CH = CH (CH2)13 COOH, trong oxynervon c acid oxynervonic cha no CH3 (CH2)7 CH=CH

(CH2)12 CHOH COOH

Trong no ngi ta cn pht hin thy cc xerebrozit c lu hunh (sulfatit), trong c nhm hydroxyl bc nht nguyn t cacbon th su ca galactoza c lin kt dng este vi acid sunfuric:

Sulfatit

Xerebron b. Gangliozit (hoc mucolipid) l nhng glicolipid cao phn t gm c acid bo (thng l acid stearic), sphingozin, galactoza v glucoza galactozamin v acid nraminic. Nhng nm gn y ngi ta cho rng acid nraminic c mt ngha rt quan trng v ngi ta coi n nh l mt cu t ca m thn kinh. Trong thin nhin, acid nraminic thng c dng cc dn xut N axetyl v N glicozyl. Do cc dn xut ny u l nhng cu t khng th thay th c ca gangliozit vn m bo chc nng bnh thng ca thn kinh. 1.4.4. Xc nh mt s ch tiu trong du m 1.4.4.1. Xc nh hm lng lipid t do 1.1.1.1.1. Y nghia Tnh cht ca du m l do thnh phn ca cc acid bo v v tr ca chng trong phn t triglyxerit quyt nh. Triglyxerit dng tinh khit khng c mu, khng mi, khng v. Mu sc, mi v khc nhau ca du l do s c mt ca cc cht km theo. Triglyxerit do khi lng phn t tng i cao nn khng bay hi ngay c trong iu kin c quay chn khng cao. nhit trn 240 250 oC triglyxerit s b phn hy thnh cc sn phm bay hi. Di tc dng ca cc enzyme lipaza, khi c nc v nhit , triglyxerit s b thy phn to thnh cc acid bo t do, do trong du m bao gi

cng c mt mt s cc acid t do. Thnh phn glyxerit ca du v m rt phc tp. S loi glyxerit c trong thnh phn du, m t hng chc n hng trm. 1.1.1.1.2. Cac phng phap xac inh lipid trong du m Khng c phng php chung no c th p dng xc nh hm lng cht bo cho cc sn phm thc phm. Ty theo hm lng cht bo c trong thc phm v tnh cht ca thc phm s c phng php phn tch khc nhau. i vi nhng sn phm m hm lng cht bo chim trn 80% (v d: du, m, b ng vt, b thc vt) ngi ta xc nh gin tip hm lng cht bo thng qua vic nh lng thnh phn khng bo ca sn phm (v d: nc, mui, casein). Tuy vy, cng c th tin hnh nh lng trc tip hm lng cht bo trong sn phm. i vi nhng sn phm m hm lng cht bo nh hn 80% th s tin hnh tch chit cht bo trong thc phm bng dung mi thch hp sau o xc nh trc tip hm lng cht bo tch chit c. 1.1.1.1.3. Xac inh ham lng lipid theo phng phap soxhlet a. Nguyn tc Phng php da vo tnh cht ha tan ca cht bo vo dung mi hu c, cht bo c chit ra khi nguyn liu sy kh bng thit b soxhlet sau tch ra khi dung mi v m ct. b. c. Ha cht, dng c Ete petrol hoc ete etylic B trch ly soxhlet Cch tin hnh Cn vo ng giy 3 - 10g nguyn liu th nghim c nghin nh v sy kh n trng lng khng i. ng giy phi c ng knh nh hn ng knh tr chit v chiu cao nh hn hoc bng 2/3 chiu cao phn tr chit tnh t y ti mp trn ca ng xi phng. y ng giy trc khi cho mu nguyn liu vo cng

nh u trn ca ng giy sau khi cho mu c lt v ph kn bng mt lp bng thm nc sch. Gi kho hoc buc bng ch hai u ng giy li. t ng giy c mu vo tru chit (chu y: kh bo nc ngi ta sy ng giy vi nguyn liu thi nghim trong tu sy chn khng hoc la CO 2 hay N2). Vi ham lng cht beo thng tinh thanh phn trm trn cht kh nn cn xac inh m cua nguyn liu. Trc khi chit, binh cu c sy kh n trong lng khng i trn ni cach thuy hoc un nong bng bong in 100 - 120W. Bng phu qua ng sinh han cho ete vi lng gp ri dung tich cua phn tru chit tinh t ay n mep trn cua ng xi phng. M nc vao ng sinh han va bt u chit. cho ete si khng qua manh, nhit cua nc trong bp cach thuy khng qua 45 - 50 oC iu chinh sao cho s ln trut ete t tru chit vao binh cu khoang 10 - 15 ln trong 1 gi (4 - 6 phut mt ln). Qua trinh chit tin hanh trong khoang 10 - 12 gi Th xem cht beo a chit hoan toan cha bng cach nho vai giot ete t u mut cua tru chit ln kinh ng h sach. Nu sau khi ete bay hi ht ma khng con lai vt cht beo nao trn kinh, thao bo ng giy ng nguyn liu, lp lai b Soxhlet va tin hanh ct thu hi dung mi. Sy binh co cha cht beo n trong lng khng i ri em cn. Khi chit bng ete etylic thi sy nhit 60 - 70 oC trong 30 phut. d. Tnh kt qu Ham lng cht beo c tinh theo cng thc sau:

Trong o: X: ham lng cht beo (%); a: khi lng binh khng (g); b: khi lng binh va cht beo (g);

m: khi lng mu thi nghim (g); w: m cua nguyn liu (%). 1.1.1.1.4. u v nhc im ca phng php soxhlet Chit soxhlet l phng php chit lin tc nn kt qu chit hon ton hn phng php chit gin on v s dng t dung mi, nhng mt hn ch l thi gian chit tng i di v khng s dng cho cc cht km bn nhit. 1.4.4.2. Xc nh ch s acid theo TCVN 6127 : 2010 1.1.1.1.5. Y nghia Qua ch s acid ngi ta c th nh gi cht lng du m. Ch s acid cng cao chng t du m km cht lng v ngc li ch s acid cng thp du cng tt v c bo qun tt. 1.1.1.1.6. Pham vi ap dung Tiu chun nay quy inh ba phng phap (hai phng phap chun va mt phng phap in th) xac inh trong du m ng, thc vt. acid c biu thi theo tri s acid hoc cach khac, theo acid c tinh theo quy c. Tiu chun nay c ap dung cho du m ng, thc vt dang th va tinh luyn cac acid beo gc xa phong hoc cac acid beo ki thut. Khng ap dung cho cac loai sap. Vi cac phng phap nay hoan toan khng c trng nn khng ap dung chung phn bit gia cac acid v c, acid beo t do va cac loai acid hu c khac. Do o, tri s acid cung gm ca acid v c co th co mt. 1.1.1.1.7. inh nghia Tri s acid la s miligam hydroxit dung trung hoa cac aixt t do co trong 1 gam cht beo. acid la ham lng cac acid beo t do xac inh theo tiu chun nay. 1.1.1.1.8. Nguyn tc

Mu th c hoa tan trong hn hp dung mi thich hp va cac acid co mt c chun bng dung dich kali hoc natri hydroxit trong etanol hoc trong metanol. 1.1.1.1.9. Thuc th Dung mi etanol (96%); Dung mi ietyl ete (hoc ter-butyl metyl ete); Hn hp dung mi (trn 2 dung dich etanol va ietyl ete vi lng th tich bng nhau); Thuc th phenolphtalein, thymolphatalein dung dich trong etanol. Dung cu, thit bi

1.1.1.1.10. -

Buret 25mL; Erlen 250mL; Becher 250mL; Cn phn tich (0.001g); Dung cu chun t ng in cc pH kt hp; Binh inh mc 1000mL.

1.4.4.2.7. Cc phng php v cch tin hanh a. Phng phap dung mi lanh s dung cht chi thi (phng phap chun) Tuy thuc vao tri s acid d kin, chon khi lng va thuc th va nng kim theo bang 1.3. Bng 1.3. Khi lng ca phn mu th v nng ca dung dch kim Tri s acid xp xi Khi lng phn mu th Nng KOH (mol/l) 0.1 chinh xac cua phep cn phn mu th (g)

Nhom san phm Du thc vt tinh luyn M ng vt

T 0 n 1

20

0.05

Nhom san phm Du thc vt th M ng vt loai ki thut Acid beo gc xa phong Acid beo ky thut

Tri s acid xp xi T 1 n 4 T 4 n 15 T 15 n 17 >75

Khi lng phn mu th 10 2.5 0.5 3.0 0.2 1.0

Nng KOH (mol/l) 0.1 0.1 0.1 0.5 0.1 0.5

chinh xac cua phep cn phn mu th (g) 0.02 0.01 0.001

0.001

Cn phn mu th theo bang trn cho vao binh erlen 250mL; Thm t t 50 100mL hm hp dung mi a trung hoa va hoa tan phn mu th bng cach lam nong nhe (nu cn); i vi cac mu co im tan chay cao, thi s dung etanol toluen. Sau khi thm cht chi thi chun bng dung dich chun kali hydroxit trong khi xoay binh lin tuc. Vic chun coi la kt thuc khi thm 1 giot kim se tao mau nhe nhng vic i mau n inh it nht 15 giy. b. Phng phap dung mi lanh s dung chun in th (phng phap chun) Cn mu theo bang 1, cho vao cc co mo 150mL. Thm t t 50 100 mL hn hp dung mi a trung hoa va hoa tan mu, lam nong nhe (nu cn). i vi cac mu co im tan chay cao, thi s dung etanol tuluen. a in cc kt hp vao hn hp vao dung mi va ni in cc vi dung cu chun t ng. Bt may khuy it nht 30 s va chun bng dung dich kali hydroxit chun trong khi vn khuy lin tuc. Ngay khi at im tng ng, ghi lai lng dung dich a s dung. c. Phng phap dung etanol nong co s dung chi thi

 cac iu kin quy inh trong phng phap nay, nu co mt cac aixt beo mach ngn thi chung la loai bay hi. Cn mt lng u mu th theo bang trn, tuy theo mau sc va tr s acid d kin cho vao binh cu th nht. un n si 50 mL etanol cha 0.5 mL cht chi thi phenolphtalein cho vao binh cu th hai. Khi nhit cua etanol vn con cao hn 70oC, thi trung hoa cn thn bng dung dich natri hydroxit hoc kali hydroxit 0.1 mol/l. Vic chun c coi la kt thuc khi thm mt giot kim se tao mau nhe nhng vic i mau n inh trong it nht 15s. Co th cn n cac th tich etanol va cht chi thi ln hn i vi cac loai cht beo co mau m. Ngoai ra, i vi cac cht beo co mau m nay, cn s dung alkali blue hoc thymolphtalein. Thm etanol a trung hoa vao phn mu th vao binh cu th nht va trn ki. un n si lng cha trong binh va chun bng dung du\ich kali hydroxit hoc natri hydroxit, lc manh binh trong qua trinh chun . 1.4.4.2.8. Tinh toan Tri s acid, Wav, hoc ham lng acid bo t do, WFFA c ghi lai nh sau: n hai ch s thp phn i vi cac gia tri t 0 n 1; n mt ch s thp phn i vi cac gia tri t 0 n 100; Ly n s nguyn i vi cac gia tri > 100; i vi cac phep tinh sau y, ham lng acid 1 beo t do ( acid) xp xi c tinh t:

WFFA = 0.5 a. Tri s acid Tri s, WAv , c tinh theo cng thc sau:
WAV =

WAV

56.1C V m

Trong o: C: nng cua dung dich chun NaOH (hoc KOH) a s dung, (mol/l); V: th tich cua dung dich chun NaOH (hoc KOH) a s dung, (mL); M: khi lng phn mu th (g). b. acid hoc ham lng acid beo t do acid hoc ham lng acid beo t do, W FFA, c biu thi bng ti l phn trm khi lng tuy thuc vao loai cht beo (xem bang 2), tinh c theo cng thc sau:

Trong o: V: th tich dung dich chun NaOH hoc (KOH) (mL); C: nng cua dung dich NaOH hoc (KOH) (mL); m: khi lng mu th (g); M: khi lng mol cua acid c chon biu din (g/mol). Bng 1.4. Chn acid bo biu th acid Loai cht beo Du da, du nhn co va cac loai du tng t Du co Cac loai du ho cai du cruciferae Tt ca cac loai du khac Biu thi theo Acid lauric Acid palmitic Acid eruxic Acid oleic Khi lng mol (g/mol) 200 256 338 282

Nu ham lng acid aruxic ti a la 5% thi acid co th c biu din theo acid oleic 1.4.4.2.9. u v nhc im ca cc phng php

V cc phng php ny khng c trng nn khng p dng chng phn bit gia cc acid v c, acid bo t do v cc loi acid hu c khc. Do , tr s acid cng gm c acid v c c th c mt. 1.4.4.2.10. So snh gia TCVN 6127 : 2010 vi TCVN 6127 : 2007 TCVN 6127 : 2010 TCVN 2127 : 2007

nh ngha: ch s acid l s miligam kali hydroxit dng trung ha cc acid bo t do c trong 1 g cht bo. Nguyn tc: mu th c ha tan trong hn hp dung Ging nhau mi thch hp v cc acid c mt c chun bng dung dch kali hoc natri hydroxit trong etanol hoc metanol. Ha cht: etanol, dietyl ete, NaOH hoc KOH, phenolphtalein. p dng cho 3 phng php: 2 Khc nhau phng php chun v 1 phng php o in th. 1.4.4.3. p dng cho 2 phng php: 1 phng php chun, 1 phng php o in th.

Xc nh ch s x phng ha theo TCVN 6126 : 2007

1.4.4.3.8. Y nghia Trong du m thnh phn chnh l acid bo v triglycerit, ty theo mi loi du m thnh phn v t l ca acid bo v triglycerit khc nhau. Qua ch s x phng ha ta c th bit c trng lng phn t trung bnh ca cc acid bo. Cc acid bo c cu to triglycerit cng ngn th ch s x phng ha cng ln (ngha l cn nhiu KOH mi x phng ha hon ton du). 1.4.4.3.2. Pham vi ap dung

Tiu chun nay quy inh phng phap xac inh chi s xa phong cho du m ng thc vt. Chi s xa phong la s o acid t do va acid este hoa co trong m va acid beo. Phng phap nay cung co th ap dung cho m ng, thc th va tinh ch. 1.4.4.3.3. inh nghia Chi s xa phong (saponification value) la s miligam kali hydroxit xa phong hoa 1 g cht beo di iu kin quy inh cua tiu chun nay. 1.4.4.3.4. Nguyn tc un si mu th vi dung dich kali hydroxit trong etanol d trong h thng co lp b sinh han hi la. Sau o chun lng kali hydroxit d bng dung dich chun clohydric. 1.4.4.3.5. Thuc th Kali hydroxit (0.5 N) trong etanol 95%; Acid clohydric (0.5 N); Dung dich phenolphtalein; Dung dich kim xanh 6B (= 2,5g/100mL) trong etanol; Cht tr si.

1.4.4.3.6. Thit bi, dung cu a. B sinh han; Dung cu un nong; Buret 25mL; Pipet 25mL; Cn phn tich; Binh non. Mu th Cn khoang 2 g mu th, chinh xac n 5 mg cho vao binh non.

1.4.4.3.7. Cach tin hanh

Phn mu th 2 g xac inh chi s xa phong t 170 n 200. i vi cac chi s xa phong khac lng phn mu th cn c thay i cho phu hp sao cho khoang mt na dung dich kali hydroxit trong etanol c trung hoa. Khi lng phn mu c nu trong bang 1.5. Bang 1.5. Khi lng mu th Chi s xa phong hoa d kin 150 n 200 200 n 250 250 n 300 >300 b. Xac inh Dung pipet ly 25,00 mL dung dich kali hydroxit trong etanol cho vao phn mu th va mt it cht tr si. Ni b sinh han vi binh, t binh ln dung cu un nong va un si t t, thinh thoang lc nhe trong sut thi gian 60 phut (hoc 2 gi) trong trng hp du m co im nong chay cao va kho xa phong hoa. Cho thm vao dung dich un nong 0.5 1 mL dung dich phenophtalein va chun vi acid clohydric cho n khi mau hng cua dung dich bin mt. Nu dung dich co mau m thi s dung 0.5 1 mL dung dich kim xanh 6B. Lam mu trng tng t nhng khng co mu. 1.4.4.3.8. Tinh toan kt qua Chi s xa phong hoa Is, c tinh theo cng thc Khi lng phn mu th 2.2 g n 1.8 g 1.7 g n 1.4 g 1.3 g n 1.2 g 1.4 g n 1.0 g

Trong o : V0: th tich cua dung dich acid clohydric tiu tn cho mu trng (mL); V1: th tich cua dung dich acid clohydric tiu tn cho mu tht (mL); C: nng cua acid clohydric (N);

m: khi lng mu (g).

1.5. Gii thiu mt s h thng chng ct t ng

1.5.1. Yu cu chung ca thit b v iu kin x l mu x l mu, ty thuc vo iu kin trang thit b, loi mu, cht phn tch, m chng ta c th la chn cc loi trang thit b v phng php x l cho ph hp. Ngy nay trn th trng c bn rt nhiu trang thit b khc nhau x l mu phn tch t n gin cho n phc tp v hon ton t ng. Tuy nhin, cc thit b i hi phi tha mn cc yu cu sau: Thc hin QA/QC trong qu trnh x l mu. Ph hp vi mi loi mu,n gin, ph thng. Khng lm mt,nhim bn mu phn tch. D chn ch no, dng c no, th cng m bo x l mu mt cch tt nht, khng lm mt mu, nhim bn mu v a cht cn xc nh v dng ph hp nht cho phng php phn tch chn. 1.5.2. Cc thit b chng ct dung mi t ng 1.5.2.1. B chit cht bo soxhlet SOX 406 Hanon

Hnh 1.1. B chit cht bo soxhlet SOX 406 Hanon Thit b phn tch cht bo hot ng da trn nguyn tc chit Soxhlet v tch hp cc chc nng nh ngm, chit, lc, nng, ngng t v thu hi dung mi.

Phm vi kim sot nhit rng v chnh xc cao, iu khin nhit t ng, m bo nhit ng nht v hot ng an ton, thit b truyn nhit l tm kim loi nng c trng ca thit b: Hot ng da trn nguyn tc chit Soxhlet v tch hp cc chc nng nh ngm, chit, lc, nng, ngng t v thu hi dung mi Phm vi kim sot nhit rng v chnh xc cao, iu khin nhit t ng, m bo nhit ng nht v hot ng an ton, thit b truyn nhit l tm kim loi nng in c c lp t khng gian chit, bo m an ninh thit b. Cc chc nng ci t thi gian Bo ng khi nhit qu cao v chc nng hn gi nhc nh c sn Ba hnh thc thng bo l m thanh bo ng, nh sng thng bo, thng bo trn mn hnh LCD Giao din phong ph :hin th ng thi nhit ci t, nhit thc t, thi gian ci t v thi gian lm nng. Nng cp kt ni tuyn tnh ca trc v kh nng dn truyn cho hot ng m nh v thoi mi. H thng kim sot thng minh tng tc gia ngi v my. S dng tm ghp chn khng kh trong trng hp nhit phng Mn hnh LCD 5.1 v h thng iu khin kt ni my vi tnh. Bng 1.6. Thng s k thut b chit cht bo soxhlet SOX 406 Hanon Model Phm vi o Cng sut Hiu sut thu hi lp li( h s bin thin) SOX 406 0.1-100% 6 mu/ m 80% 1%

Model Khi lng mu Th tch dung mi Nhit chnh xc in p Cng sut

SOX 406 0.5 15 g 80 mL Nhit phng + 5oC -280oC 1o C 220V / 50HZ 1000 W

1.5.2.2. H thng chit B-811

Hnh 1.2. H thng chit B-811 L h thng thun tin v linh hot nht trong cc h thng chit t ng vi bn k thut chit khc nhau. Thc hin chit Soxhlet chun, chit Soxhlet m, chit nng hoc chit dng lin tc mi qu trnh chit u c thc hin hon ton t ng v c kim sot. Thm vo , n lm vic trong iu kin kh tr hon ton. Thit b ny c dng cu hnh chun v cu hnh LSV cho cc mu th tch ln (phn tch lng vt). c trng ca thit b

Thc hin cc k thut chit: Chit nng, chit Soxhlet chun, chit Soxhlet nng, v chit dng lin tc Sp xp t ng: Bng in t sp xp vic thc hin ba qu trnh (chit, ra gii, lm kh) ca 4 mu ng thi song song. Thc hin nhanh qu trnh chit: 2 ngun nhit c gn trn mi b chit, v nhit c truyn mt cch ti u cho php s dng cc loi dung mi c nhit si cao. Hn na, vic kim sot bng b cm bin quang hc gip ngi s dng c th tnh ton thay i dung mi lm tng hiu sut chit v tit kim dung mi.

Vn hnh an ton: Cc ch s v nc lm mt, lng dung mi, v ngun nhit u c gim st trc tip. B dng c th nghim c sn xut c bit m bo ghp ni vi nhau cht kht, ngoi ra vn c mt tm chn bo v ton b h thng.

Qu trnh lm kh thch hp vi mu: Trong trng hp mu khng chu nhit th dch chit s c c ch bo v. Nu mu d b oxi ha th s c chit v lm kh trong mi trng kh tr.

Mu lun c gi tinh khit: Tt c cc dng c tip xc vi mu u c m bo khng lm nhim bn cho cho mu Bng 1.7. Thng s k thut ca h thng chit B-811 Moden B 811 230 V 50/60 Hz 1250 W 120 mL 312 mL 39 mL 150 mL

Ngun Tn s Cng sut Th tch bnh chit Chiu di ng ngng ng knh b gi mu Th tch ng thy tinh cha mu

Th tch cc dung mi Lng nc tiu th ti a cho lm mt Moden p lc nc ti a Kch thc (WxHxD) Trng lng Giao din

150 mL 60 l/ gi B 811 5 bar 600x980x290 mm 32 kg Rs 232

1.5.2.3. B trch bo Soxhlet SER 148/6

Hnh 1.3. B trch bo Soxhlet SER 148/6 Thit b c thit k theo nguyn l chit dung mi Randall vi u im l thi gian chit nhanh v hiu qu hn so vi nguyn l Soxhlet. c trng ca thit b u lc c ch to bng s cotton cellulose vi chiu dy 1mm gip dung mi d dng i qua vi tng hiu qu chit. ng dng chit cc mu thc phm, thc n chn nui, cht ty ra, cao su, nha, dc phm, t nhm xc nh hm lng cc cht bo, cht hot ng bn mt, nha v thuc tr su.

Thit b c thit k t cc tiu chun AOAC, TAPPI, UNI, EPA, ASTM, APHA, AWWA, WEF. Cu trc bng thp khng g sn ph Epoxy c kh nng chu n mn ho cht. Hai mn hin th LED hin th gi tr nhit lm vic v gi tr ci t. iu khin nhit bng 2 b vi x l v u o nhit Pt100, gip thit b t tiu chun IP55. Bng 1.8. Thng s k thut ca B trch bo Soxhlet SER 148/6 Moden S v tr c mu Th tch cc chit Khi lng mu Th tch dung mi Nhit hot ng T l thu hi dung mi Tiu tn nc lm mt Cng sut Ngun in Kch thc Khi lng SER 148/6 6 150 mL 0.5 15 g 30 100 mL 100 2600C 50 75% 8l / pht 950 W 230 V, 50 Hz 700x620x390 mm 40 kg

1.5.2.4. B chit Soxhlet/chit nng E-812/ 816

Hnh 1.4. B chit Soxhlet/chit nng E-812/ 816 c thit k cho nhng ng dng trong lnh vc thc phm v thc n gia sc ph hp vi phng php AOAC. Chng l h thng chit Soxhlet hon ton t ng (E-812/816 Sox) hay cu hnh chit nng (E-812/816 HE) c dng chit nng t ng theo phng php Randall hay Goldfisch. c trng ca thit b E-812/E-816 Sox: Chit Soxhlet t ng vi 2 hay 6 v tr

Thit b c o ny cho php p dng cc k thut chit lng-rn m khng b mc kt trong vic pht trin phng php v a ra c mt lng ln cc thng s c thtychnh. Tp trung vo nhng k thut chit ph bin, b chit E - 812, E - 816 SOX E-812/816 lun HE: sn Chit sang nng t cho ng mi vi ch 2 hay 6 v chit. tr

Thit b a nng ny cho php p dng cc k thut chit lng-rn. La chn b chit model HE vi 2 hay 6 v tr chit nng t ng theo Randall hoc Goldfisch cho vic xc nh cht bo th hoc tng cht bo Bng 1.8. Thng s k thut ca b chit Soxhlet/chit nng E-812/ 816 E - 812 Sox Ngun Cng sut tiu th Tn s Nhit Chiu cao m E - 816 Sox

100120 V/220240 V 10 % 700/1200 Watt 1950/1200 Watt 50/60 Hz Ch s dng trong nh, 5 40C Ln n 2000 m m tng i ti a l 80 % nhit ln n 31C v gim tuyn tnh xung n 50 % 40 C. 130 mL 130 mL

Th tch bnh nn

Th tch bnh ng mu Th tch bung Soxhlet thy tinh 190 mL E - 812 Sox Mc nc lm lnh ti a cn dng p sut nc ti a E - 812 Sox Kch thc (W x H x D) Trng lng 1.5.2.5. B thy phn E-

115 mL E - 816 Sox 72 l/h 4 bar E - 816 Sox 635 x 776 x 456 mm 36 kg 416

275 x 776 x 456 mm 21 kg

Hnh 1.5. B thy phn E-416 B thy phn E - 416 thy phn acid nhanh v an ton cho nhiu mu trong cng mt thi gian. Qu trnh thy phn acid l mt phn khng th thiu ca qu trnh chit theo phng php Weibull-Stoldt v c yu cu trong mt s phng php AOAC xc nh cht bo c trong thc phm nh pho mt, hi sn, nc st, tht c trng ca thit b Xc nh cht bo hiu qu

Kt hp l tng vi b chit B - 811: Khi xc nh hm lng cht bo theo phng php Soxhlet, khng phi lc no thu c ton b lng cht bo bng cch chit trc tip. Trong trng hp ny, thy phn trc khi chit l rt cn thit (theo Weibull-Stoldt). B thy phn E - 416 hp th ton b lng acid sinh ra vi thi gian lc nhanh nht. Su mu xc nh c thc hin ng thi. Cc tube mu thy tinh c gn trc tip vo h thng chit sau khi sy kh. Bng 1.9. Thng s k thut ca B thy phn E - 416 Moden S v tr gia nhit Th tch tube mu thy tinh Dng tiu th (220 V) Cng sut tiu th Ngun Kch thc (WxHxD) Trng lng E - 416 6 60 mL 5A 1100 W 220 240 V 275 600 570 mm 13,5 kg

CHNG 2: NI DUNG THC NGHIM

2.1. Mc tiu nghin cu

Kho st hiu sut chng ct trn h thng chit lng lng v chng ct bn t ng. Kho st mt s ch tiu trong lipid, kim sot quy trnh phn tch ng gi cht lng du m.

2.2. Thit b - ha cht

2.1.1. Thit b H thng chit lng lng v h thng chng ct bn t ng; Cn phn tch c chnh xc 0.0001 g; Chn s; T sy t nhit 300 5oC c b phn iu chnh nhi ; Bnh ht m dng cho phn tch; Burrette 25mL c khong chia vch n 0.1 mL; Cc dng c thy tinh thng dng trong phng th nghim.

2.1.2. Ha cht B, lp xng, m hoc du thc vt (Vit Nam); Dimetyl ete khng cha peroxit c tinh khit cao (Trung Quc); Ete du ha c tinh khit cao (Trung Quc); Cht tr si bt (Trung Quc); Than hot tnh v silicagel (Trung Quc); Dung dch KOH 0.5 N trong cn (Trung Quc); Dung dch KOH 0.1 N pha trong nc (Trung Quc); Dung dch HCl 0.5 N trong nc (Trung Quc); Ch th phenolphtalein 1 % pha trong cn (Trung Quc).

2.3. Ni dung nghin cu

2.3.1. Nguyn tc thit k Da vao s cu to, nguyn tc hoat ng cua h thng thuy phn E - 416 la thit bi chng ct ban t ng c s dung xac inh cht beo co trong thc phm nh phosmat, hi sn, nc st, tht chung ti a khao sat va chon ra c cac b phn chinh cn thit cua thit bi tao nn h thng chng ct ban t ng. Nhng b phn chinh cua thit gm: bp un cach thuy, binh cu, ng soxhlet, ng sinh han, ng dn khi, binh hp phu. 2.3.2. Ban ve thit k

Chu thich: 1) Bp un cach thuy 2) Binh cu 3) Erlen 4) ng soxhlet 5) ng sinh han 6) Co ni 7) ng dn khi 8) Binh hp phu 9) ng dn nc

Hinh 2.1. Mt trc cua m hnh thit k

Hinh 2.2. Mt sau cua m hnh thit k

Hinh 2.3. Mt bn cua m hnh thit k

CHNG 3: KT QUA V BN LUN

3.1. Gii thiu v h thng chit long long va chng ct ban t ng

3.1.1. Cu tao cua thit bi

Hinh 3.1.Mt trc cua m hnh thit b

Hinh 3.2. Mt sau cua m hnh thit b

Hinh 3.3. Mt sau cua m hnh thit b Thit bi c thit k hoan chinh nh hinh 3.1. bao gm cac b phn chinh sau: Bp un cach thuy; Binh cu; Erlen; ng soxhlet; ng sinh han; ng dn khi; Binh hp phu.

3.1.2. Bp un cach thuy

Bp un cach thuy dung tng nhit trong qua trinh un si dung mi vi cac thng s ky thut: Vt liu cu tao bng mt thanh thep hinh ch U; Ngun in: 220V.

Hinh 3.4. Bp cch thy 3.1.3. H thng sinh han

Hinh 3.5. ng sinh han H thng sinh han c cu tao bng thuy tinh c nham, bn trong co ng thuy tinh xon nho, c thit k phu hp cho vic lam lanh khi trong qua trinh chng ct. 3.1.4. H thng soxhlet H thng soxhlet c cu tao bng thuy tinh c nham, thch hp cho qu trinh chit.

Hinh 3.6. H thng soxhlet 3.1.5. Binh cu Binh cu c cu tao bng thuy tinh c nham, chiu nhit cao ln ti 400oC, c thit k phu hp cho vic un nong dung mi va am bao an toan trong qua trinh x li mu. Binh c gn vi h thng soxhlet a dung mi cho qua trinh x li mu, am bao an toan khi x li mu.

Hinh 3.7. Binh cu 3.1.6. Binh hp thu Thit bi thich hp dn khi c cu tao bng thuy tinh, chng n mon hoa cht, cha cht hp thu hp thu khi bay ra. Cac b phn c ni vi nhau bng ng thuy tinh. Nh vy ma co th tranh khoi bi h va thoat khi ra ngoai.

Hinh 3.8. 3.1.7. ng dn khi

Binh hp thu

ng dn khi c t silicol co ng kinh 5 8 mm va mt trong cua ng phai trn.

Hinh 3.9. ng dn khi