Sc k kh ghp khi ph v mt s ng dng (GC/MS-Gas Chromatography Mass Spectometry)

Sc k kh ghp khi ph (GC/MS_Gas Chromatography Mass Spectometry) l mt trong nhng phng php sc k hin i nht hin nay vi nhy v c hiu cao v c s dng trong cc nghin cu v phn tch kt hp. Thit b GC/MS c cu to thnh 2 phn: phn sc k kh (GC) dng phn tch hn hp cc cht v tm ra cht cn phn tch, phn khi ph (MS) m t cc hp phn ring l bng cch m t s khi. Bng s kt hp 2 k thut ny (GC/MS_Gas Chromatography Mass Spectometry), cc nh ho hc c th nh gi, phn tch nh tnh v nh lng v c cch gii quyt i vi mt s ha cht. Ngy nay, ngi ta ng dng k thut GC/MS rt nhiu v s dng rng ri trong cc nghnh nh y hc, mi trng, nng sn, kim nghim thc phm Sc k kh (GC_Gas Chromatography) Sc k kh c dng chia tch cc hn hp ca ha cht ra cc phn ring l, mi phn c mt gi tr ring bit. Trong sc k kh (GC) chia tch xut hin khi mu bm vo pha ng. Trong sc k lng (LC) pha ng l mt dung mi hu c, cn trong GC pha ng l mt kh tr gng nh helium. Pha ng mang hn hp mu i qua pha tnh, pha tnh c s dng l cc ha cht, ha cht ny c nhy v hp th thnh phn hn hp trong mu. Thnh phn hn hp trong pha ng tng tc vi pha tnh, mi hp cht trong hn hp tng tc vi mt t l khc nhau, hp cht tng tc nhanh s thot ra khi ct trc v hp cht tng tc chm s ra khi ct sau. l c trng c bn ca pha ng v pha tnh, hn na qu trnh chia tch c th xy ra bi s thay i nhit ca pha tnh hoc l p sut ca pha ng. Ct trong GC c lm bng thy tinh, inox hoc thp khng r c kch thc, kch c rt a dng. Ct ca GC di c th l 25m, 30m, 50m, 100m v c ng knh rt nh, bn trong ng knh c trnh bng mt lp polimer c bit nhphenyl 5% + dimetylsiloxane polymer 95%), ng knh ct thng rt nh ging nh l mt ng mao dn. Thng thng ct c s dng l semivolatile, hp cht hu c khng phn cc nh PAHs, cc cht trong hn hp c phn tch bng cch chy dc theo ct ny. Mt cht chia tch, ra gii phng i ra khi ct v i vo u d. u d c kh nng to ra mt tn hiu bt k lc no, khi pht hin ra cht cn phn tch. Tn hiu ny pht ra t my tnh, thi gian t khi bm mu n khi ra gii gi l thi gian lu (TR). Trong khi cc thit b chy, my s a ra cc biu t cc tn hiu nh hnh 1. y gi l sc , mi mt peak trong sc s miu t mt tn hiu to nn khi cht gii hp t ct sc k v i vo u d detector, trc honh biu din thi gian lu v trc tung biu din cng ca tn hiu, trong hnh 1 mi nh (peak) biu din mt cht ring l, cht ny c tch t hn hp mu phn tch, peak c thi gian lu (TR) 4,97 pht l dodecane, 6.36 pht l biphenyl, 7.64 pht l chlolobiphenyl, 9.41 pht l hexadecanoic acid methyl ester. Nu trong cng iu kin sc k nh nhit , loi ct gng nhau th cng cht lun c thi gian lu ging nhau, khi bit thi gian lu ca hp cht th chng ta c th chp nhn c nhy ca n. Tuy nhin, cht c tnh cht ging nhau th thng c thi gian lu ging nhau.

Hnh 1: sc ca sc k kh

Khi ph: Khi ph c dng xc nh mt cht ha hc da trn cu trc ca n. Khi gii hp cc hp cht ring l t ct sc k, chng i vo u d c dng in ion ha (mass spectrometry). Khi , chng s tn cng vo cc lung, do chng b b thnh nhng mnh vn, nhng mnh vn ny c th ln hoc nh; Nhng mnh vn thc t l cc vt mang in hay cn gi l in, iu ny l quan trng bi v cc ht cn trng thi tch in th mi i qua c b lc. Cc khi nh chc chn, khi ca mnh v c chia bi cc vt mang gi l t l vt mang khi (M/Z); Hu ht cc mnh vn c in tch l +1, M/Z thng miu t cc phn t nng ca mnh vn.Nhm gm c 4 nam chm in gi l t cc (quadrapole), tiu im ca cc mnh vn i xuyn qua cc khe h v i vo u d detector, t c c thnh lp bi phn mn chng trnh v hng cc mnh vn i vo cc khe ca khi ph. Phn tch kt qu My tnh s ghi li cc biu ca mi ln qut. Trc honh biu din t l M/Z cn trc tung biu din cng tn hiu ca mi mnh vn c qut bi u d detector. y l th ca s khi. Lm th no phn tch cc kt qu t my tnh? Di y l mt hnh khi ph. Trc X l khi lng cn trc Y l s lng. Mi ha cht ch to ra mt m hnh duy nht, ni cch khc mi cht c mt du vn tay nhn dng, da trn m hnh ion ca n. Trn hnh ta thy phn t ban u c khi lng l 5. Trn s khi ph ht ln nht ny c gi l ion phn t (molecular ion). Cc ht nh hn c khi lng 1,2,3 v 4 c gi l cc ion phn mnh (fragment ions). Trong trng hp v d trn ta thy cc phn t ca cht ny c xu hng b ph v thnh cc t hp 1-4 hn l 2-3. Cc nh nghin cu c th so snh khi ph thu c trong th nghim ca h vi mt th vin khi ph ca cc cht c xc inh trc. Vic ny c th gip h nh danh c cht (nu php so snh tm c kt qu tng ng) hoc l c s ng k mt cht mi (nu php so snh khng tm c kt qu tng ng).

Trong hnh 2, hnh nh khi cao nht l dodecane, phn nm ca GC/MS n ging nh l mt th vin hnh nh dng nhn ra cc cht cha bit tn ti trong hn hp mu. Th vin ny c th so snh hnh nh khi t thnh phn ca mu vi hnh nh khi trong th vin ca my.

Hnh 2:

Mass-spectrum

Sc k kh ghp khi ph (GC/MS_Gas Chromatography Mass Spectometry) Sc k kh ghp khi ph (GC/MS) c th phn tch cc hn hp ha cht phc tp nh khng kh, ncNu trong mu c mt cht l xut hin, khi ph c th nhn dng cu trc ha hc c nht ca n (ging nh vic ly du vn tay). Cu trc ca cht ny sau c so snh vi mt th vin cu trc cc cht bit. Nu khng tm ra c cht tng ng trong th vin th nh nghin cu, c th da trn cu trc mi tm c pht trin cc tng v cu trc ha hc. Ni cch khc, nh nghin cu thu c 1 d liu mi v c th ng gp vo th vin cu trc ni trn, sau khi tin hnh thm cc bin php xc nh chnh xc loi hp cht mi ny.

Khi GC kt hp vi MS, n s tr thnh 1 my phn tch a nng, cc nh nghin cu ha hc c th ha tan hn hp cc hp cht hu c, tch chit v bm vo my nhn dng chng, hn na cc nh nghin cu cng xc nh nng ca mi thnh phn ha cht. Hnh 3 s m t 3 chiu (di, rng, su) khi GC kt hp vi MS.

Hnh 3: M t kt qu ca phn tch qua h thng sc k kh khi ph 3D

Mt s ng dng ca sc k kh ghp khi ph Khc vi cc my phn tch d lng khng sinh nh sc k lng ghp khi ph (LC/MS/MS), th sc k kh ghp khi ph phn gii cao (HRGC/HRMS), GC/MSN sc k ghp khi ph c ng dng phn tch cc c cht trong nc tng, nc mm (3 MCPD...); Nghin cu chit xut v xc nh thnh phn cc cht ha hc, c cht, khng sinh, nh gi tn lu ca ha cht dit cn trng khc nhau trong cc vt liu hoc hp cht khc nhau.

Ngy 04/11/2008 CN. Phm Thanh Hin v Ths.Bs.Hunh Hng Quang (dch & tng hp) ________________________________________________________________________

H thng sc k kh ghp khi ph u d Ion Trap

H thng GCMS Thermo Polaris Q c kt hp gia my sc k kh Ultra Trace GC v u d khi ph by ion Polaris Q vi h b phn bm mu CompiPAL c kh nng phn tch nhn danh v nh lng nhiu loi hp cht hu c trong cc nn mu khc nhau.

1. Nguyn tc hot ng h thng sc k kh ghp khi ph (GCMS Gas Chromatography Mass Spectrometry) Tng t nh cc h thng sc k kh khc, h thng sc k kh ghp khi ph cng bao gm cc b phn: ngun cung cp kh, l ct, b phn tim mu, ct phn tch, u d, b phn ghi nhn tn hiu, v b phn in d liu phn tch; trong , u d l u d khi ph.

S cu to u d khi ph

Cc cu t ca mu sau khi tch ra khi ct mao qun s i vo trong u d khi ph. Ti y, ty thuc vo bn cht ca cht cn phn tch, s din ra qu trnh ion ha vi cc kiu ion ha khc nhau (API, ESI hay APPI), sau cc ion c ghi nhn bi u d. 2. Cu to u d khi ph u d by ion (Ion trap) H thng GCMS Thermo Polaris Q bao gm bm chn khng, b bm mu t ng (CompiPAL), my sc k kh Trace GC Ultra, u d khi ph by ion Polaris Q. u d Polaris Q gm c bn b phn chnh nh sau: Ngun ion ha ti p sut kh quyn (API). H quang hc ion (ion optics). B phn tch khi (mass analyzer). H thng pht hin ion (ion detection system)

Cu to u d khi ph by ion

3. ng dng h thng Thermo Polaris Q Phn tch d lng PCBs, PAHs, trong cc nn mu thc phm, mi trng, nc, theo yu cu ca cc c quan qun l trong v ngoi nc. Phn tch cc ha cht POPs (Persistent Organic Pollutants) trong mi trng, thc phm, Phn tch cc d lng thuc tr su trong thc phm, thy hi sn nh Trifluralin, Chlorpyrifos, vi kh nng pht hin p ng yu cu kht khe ca cc nc Nht, chu u, Phn tch cc c cht trong thc phm (3-MCPD, Histamin, Urea,) Phn tch cc hormone tng trng trong cc nn mu tht, thc n chn nui nh hc beta-agonist (Clenbuterol v Salbutamol), Testosterol, DES, h tr cc c quan chc nng trong cng tc kim sot cht lng v bo m v sinh an ton thc phm ca cc sn phm lu hnh trn th trng.

H thng GCMS Ion trap Thermo Polaris Q

Phn tch cc cht thuc nhm Phthalate (c bit l DEHP) trong cc nn mu thc phm, thi nhim t bao b, theo yu cu ca B Y t v cc c quan qun l khc. Phn tch Glyphosate trong cc sn phm go trong vic kim sot cht lng nng sn xut khu sang chu u. Phn tch cc cht thuc nhm Nitroimidazole, thuc dit nm (Propiconazole, Hexaconazole, Difenconazole) trong thy sn, tri cy v cc loi rau qu. Phn tch 22 hp cht amin thm sinh ra do t thuc nhm azo trong sn phm dt may theo quy nh ca B Cng thng (QCVN 01:2010/BCT). Phn tch nhn danh, nh tnh cc tinh du v cc hp cht hu c khc. (Ngun: Phng Phn tch Sc k)

+H thng sc k kh ghp khi ph u d Ion Trap

H thng GCMS Thermo Polaris Q c kt hp gia my sc k kh Ultra Trace GC v u d khi ph by ion Polaris Q vi h b phn bm mu CompiPAL c kh nng phn tch nhn danh v nh lng nhiu loi hp cht hu c trong cc nn mu khc nhau.

1. Nguyn tc hot ng h thng sc k kh ghp khi ph (GCMS Gas Chromatography Mass Spectrometry) Tng t nh cc h thng sc k kh khc, h thng sc k kh ghp khi ph cng bao gm cc b phn: ngun cung cp kh, l ct, b phn tim mu, ct phn tch, u d, b phn ghi nhn tn hiu, v b phn in d liu phn tch; trong , u d l u d khi ph.

S cu to u d khi ph

Cc cu t ca mu sau khi tch ra khi ct mao qun s i vo trong u d khi ph. Ti y, ty thuc vo bn cht ca cht cn phn tch, s din ra qu trnh ion ha vi cc kiu ion ha khc nhau (API, ESI hay APPI), sau cc ion c ghi nhn bi u d. 2. Cu to u d khi ph u d by ion (Ion trap) H thng GCMS Thermo Polaris Q bao gm bm chn khng, b bm mu t ng (CompiPAL), my sc k kh Trace GC Ultra, u d khi ph by ion Polaris Q. u d Polaris Q gm c bn b phn chnh nh sau: Ngun ion ha ti p sut kh quyn (API). H quang hc ion (ion optics). B phn tch khi (mass analyzer). H thng pht hin ion (ion detection system)

Cu to u d khi ph by ion

3. ng dng h thng Thermo Polaris Q Phn tch d lng PCBs, PAHs, trong cc nn mu thc phm, mi trng, nc, theo yu cu ca cc c quan qun l trong v ngoi nc. Phn tch cc ha cht POPs (Persistent Organic Pollutants) trong mi trng, thc phm, Phn tch cc d lng thuc tr su trong thc phm, thy hi sn nh Trifluralin, Chlorpyrifos, vi kh nng pht hin p ng yu cu kht khe ca cc nc Nht, chu u, Phn tch cc c cht trong thc phm (3-MCPD, Histamin, Urea,) Phn tch cc hormone tng trng trong cc nn mu tht, thc n chn nui nh hc beta-agonist (Clenbuterol v Salbutamol), Testosterol, DES, h tr cc c quan chc nng trong cng tc kim sot cht lng v bo m v sinh an ton thc phm ca cc sn phm lu hnh trn th trng.

H thng GCMS Ion trap Thermo Polaris Q

Phn tch cc cht thuc nhm Phthalate (c bit l DEHP) trong cc nn mu thc phm, thi nhim t bao b, theo yu cu ca B Y t v cc c quan qun l khc. Phn tch Glyphosate trong cc sn phm go trong vic kim sot cht lng nng sn xut khu sang chu u. Phn tch cc cht thuc nhm Nitroimidazole, thuc dit nm (Propiconazole, Hexaconazole, Difenconazole) trong thy sn, tri cy v cc loi rau qu. Phn tch 22 hp cht amin thm sinh ra do t thuc nhm azo trong sn phm dt may theo quy nh ca B Cng thng (QCVN 01:2010/BCT). Phn tch nhn danh, nh tnh cc tinh du v cc hp cht hu c khc. (Ngun: Phng Phn tch Sc k)