[application note] AC QUIT Y U P L C / E L S / U V: ONE M E T HO DO LOGY FO R F FA, FAM E AND TAG ANA LYSIS O F BIO D I E S E L

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1 [ppto ot] AC QUIT Y U P L C / E L S / U V: ONE M E T HO DO LOGY FO R F FA, FAM E AND ANA LYSIS O F BIO D I E S E L Ptr J. L A J. D Go Wtrs Corporto, Mor, MA U.S. INT RODUCTION Bos, tr o or wt oss s u, s st trst us o vrot tors, t upsur ptrou prs, tvs ovrt ts or ts us. 1-4 Fro 2004 to 2005, os prouto pty t Ut Stts rs ro 0.1 o to 1.1 o tos. I 2004, t prouto pty t Europ Uo ws 2.3 o tos s xpt to rs to 4 o tos Bos prout strs v sts vrous outrs, u t U.S. (ASTM D 6751), EU (EN14214 EN590) Brz (ANP 255). 1-4 D s tty ty strs (FAME) o s os t, os s ooy prou y trsstrto o tryyros () wt to t prs o tyst (Fur 1). Pott otts o os prouts u urt, rto trts [oo-yyros (MAG) yyros ()], rto y-prouts (yro), r tty s (FFA) ro uwt yroyss rtos. Cott os to svr pros trus, utoos rps su s posts, tr o, u trorto. 1-2 To vo ts t prouto sttus s otor to roz orrt y pros t ry st so to quty t otts t os prout. 1,2,5,6 Bot GC HPLC r us to yz os ts otts 1,2,8-13 typy rqur utp tos wt rt xprt otos to rtrz os purts. For xp, FAME yz y GC. T yss rqurs GC to wt sp tprtur (350 C) st pry ou rvtzto o t o-vot otts (FFA, MAG ) or to. Drvtzto s t-osu ot wys qutttv. 1,2,8 Most ovto HPLC tos v 30 to 80 ut ru t us ot sovts tt r ow ros, rstrt, sots prot ortors Ts ppto ot ouss o t tty ty str os prouto srs rp yss to us t Wtrs ACQUITY UPLC syst wt t Potoo Arry (PDA) Evportv Lt Sttr () ttors wt owr toxty sovts, totr 2-propo, s t o ps. Ts 12-ut UPLC to s rsouto sstv sprto o os sto, rto trts, yro, FFA t prouts (FAME) s xprt. T ty to quy ry yz ts rt opots tt otor t prouto prosss to prov t y. Wt ttr otro o prout quty, t os o sussu orzto rt pt r sr to r. EX PERIMENTAL Sp prprto Bos ws sytsz us t t os to wt suprrt r soy o, rt r M N. 14 A s porto o os ws ut wt IPA t souto ws tr wt 0.45 µ PVDF syr tr (WAT200531) to 12 /L souto or UPLC yss. Bos rt strs (T 1) wr purs ro S-Ar TCI Ar ssov 2-propo (IPA) to sto soutos. T sto soutos wr urtr x to str souto ot 0.5 /L o strs 0.7 /L o soy o. LC otos LC syst: Wtrs ACQUITY UPLC wt ACQUITY UPLC PDA/D Sotwr: Epowr 2 (u 2154) Dtto: PDA 195 to 300 Sp rt: 20 pts/s Ftr rspos: st W ws: 2-propo (600 µl)

2 [ppto ot] Stro ws: 2-propo (600 µl) S ws: 90:10 wtr/ch 3 CN (5 ) Cou tp.: 30 C Ito: 2 µl (u oop) Mo ps A: CH 3 CN Mo ps B: 2-propo Cou: ACQUITY UPLC BEH C x 150 Mto o: 22 uts Fow rt: 0.15 L/ Lr rt: 10 to 90% B 22 uts Mto two: 12 uts Fow rt: 0.17 L/ Grt: T () %B Curv prtrs G: 500 Nuzr: Coor N2 s prssur: 40 ps Dt rt: 20 pt/s Drt tu tp.: 55 C T ostt: 0.1 RESULTS AND DISCUSSION Fur 1 ustrts t trsstrto yroyss rtos o strs, t rt rtos vov os prouto us s os t s sto. Nurous orts v to optz t prouto prosss su tt t ovrso o to FAME s xz w t otts t os prout r z. 1,2,5,6 S otts rs ur propr prouto pross or ur poor stor otos, st r yt to us t utp sts to rs t possty or prout ur. W prvousy rport tt t -prssur u ous o UPLC syst rsouto sstv, st sprto o opots o s os wt t ACQUITY UPLC s prt Trsstrto rtos Stp 1 OCOR' OCOR" Tryyro () Stp 2 Stp 3 MAG OCOR" (1.7 µ) ou tooy us owr toxty sovts, totr 2-propo s t o ps. 15,16 T UPLC to ws pp to rtrz t o os t str souto ot 18 os rt yt strs soy o. T 1 sts t s CAS urs o t strs us ts stuy u yro (1), sx FAME (4, 7, 10, 11, 13 15), sx FFA (2, 5, 8, 9, 12, 14) two MAG (3, 6), (16), two (17, 18) soy o (19). Furs 2 3 sow 210 PDA xtrt rotors o t os t str souto ot us 22-ut r rt to wt 2.1 x 150 BEH C 18 ou. My w sprt ps r osrv t xp rotors (Fur 2). Most o t r t y opr tr rtto ts wt t strs (Fur 3 T 1). + R + R + R tyst tyst tyst OCOR" Dyyro () R = M Not: Et uto r so rport or trsstrto Hyroyss o Estrs, MAG FAME + H 2 O tyst Mooyyro (MAG) Gyro Gyro + + R'COOM Ftty A Mty Estr (FAME) + R''COOM (FAME) + R'''COOM (FAME) R'CO R''CO R'''CO FFA + M

3 [ppto ot] Exp Fur 2. rotor o o os (12 /L) ro soy o Muts M Muts Exp Fur 2. (210 ) rotor o o os (12 /L) ro soy o Muts M Fv FAME (4, 7, 10, 11 13), t prouts o trsstr-, 1,3-ooy-r-yro p, yry trot to o soy o, r w sprt ro otts wt p. rtto ts tw 3.7 to 7 uts s sow y t or ps o t rotor: ty ot p, ty ot p, ty ot ty ptt o-ut p, ty strt p.17 Gyro (1), MAG (3 6), (16), (17) t v FFA ro uwt yroyss rtos (2, 5, 8, 9, 12) r so w sprt: yro p, 1-ooy-r-yro o o-ut p, o 1-ooy-r-yro p, o pt p, str p T ps wt rtto ts or t 12 uts t w wt tt o opots o soy o. T ps v rtto t tw 7 to 12 uts r ost y rto trts,. Coprso o rtto t o strs sows tt t sprto s s o t ur o y s, t t ur o ou os (Fur 3 T 1). T yts wt wr y s ut rst. Ao yts wt t s ur o y s, tos wt sortr t r

4 [ppto ot] ur o usturt os 0.80 FFA wt usturt os ut rr. T ty strs 0.40 v stro sor t 210 us to 160 uwt yroyss rtos. 80 prsy otor t prorss o trsstrto rtos PDA xtrt rotor. tors o soy o t sy to osrv Ts 210 xtrt ro- 1 Muts Fortuty, ow- sor opots o v st rspos ur t tto otos (Fur 3). Ts ustrts t vu o o PDA ttors wt ACQUITY UPLC syst or os Fur 3. (210 ) rotors o t str souto us rt to 1: soy o (0.7 /L), FFA, FAME, MAG, (0.5 /L ). yss. Wt s rotorp ru, t o- sor opots yz sutousy. Bus t rt opots o os osrv s xprt us ts UPLC toooy, t s t ppro to otor t trsstrto sttus or pross opt- ID 1 N Gyro CAS No P L zto. Iy, t-o rto pross, ps o 2 Lo sto sou rs w t ps o MAG, FAME 3 1-Looy-r-yro ppr t rotors. Mw, t p tsty o 4 Mty ot MAG sou strt to rs w sustt out 5 Lo o s osu. 6 1-Ooy-r-yro Mty ot O Pt ro t rotors. By pott t p tsty o ro- 10 Mty ot tors st rto t, tr s t pott to sy 11 Mty ptt otor t rto ts. Dur t prouto prosss, T p tsty o FAME w otu rs wrs t ps o, MAG rs tvy sppr 12 Str y stur pps, t ou osrv or y 13 Mty strt ot PDA tto. I to, t o ps us 14 Ar t urrt xprt s opt wt ss sptrotry 15 Mty rt 17 ttors,, to ot to strutur ts. 16 1,3-ooy-r-yro I w vop os prouto pross, r y rs o t t o t rtv out o FAME, FFA rsu tot to rt sos. Ur su rusts, to ,2,3-trooyyro Gyry trot Soy o T 1. Bos rt strs p.

5 [ppto ot] Fur 4. rotor o o os (12 /L) ro soy o Muts M Fur 4. (210 ) rotor o o os (12 /L) ro soy o. Exp 0.06 Muts M t prrr to sprt FAME ro FFA ow t 3. Howvr, wt t 12-ut to, t opots opots to ut totr t t o rotor s t ut t 9.5 to 11 uts r. T 12-ut rt rsu tot sy uuousy qut. to urtr rs t trouput o os prout T 22-ut r rt UPLC to ws optz or yss. t yss o sust o, FAME FFA rt opous or rsouto trouput. Furs 4 5 sow PDA xtrt 210 rotors o t o os t str souto ot us 12-ut rt to. CONC LUSION T Wtrs ACQUITY UPLC syst wt PDA ttors s syst or t yss o os or otts. It s rp, sstv, rsouto sprtos ur T rst uts o t 12-ut rotor r ry pross otor o prout s xprt. T t to tos o t 22-ut to sow Furs 2 sprto s svr ts str t ovto HPLC wtout us tox ot sovts.

6 [ppto ot] o soy o Fur 5. (210 ) rotors o t str souto us rt to 2: soy o (0.7 /L), FFA, FAME, MAG, (0.5 /L ). Muts 1 1 A to vu or ppy UPLC tooy or os 7. S.K. Kr t, JAOCS. 2004, 81 (5): yss s ru sovt osupto zrous sovt 8. V.G. Dourtoou t. JAOCS. 2003, 80 (3): wst spos, rsut ost sty ts. By poy 9. P. Sr t. J. Crotor. 2002, A (974): t optry tto o vportv t sttr- 10. V. M. Kpous t. J. Crotor. 1986, 366: , or orto pr rotorp ru ws ot, tus 11. C.A. Dors, JAOCS , 79 (8): , rty rs proutvty. Otr ustrs su s r- 12. M. Rou-N t. Ayt C At. 2004, 513: utur s vopt, pptos, oo, ost prso r wt trst s os FFA ou so t ro ts toooy.15, LCGC, T Appto Notoo. 2006, Spt 1: ttp://t-os.o/ 15. P. J. L, C. H. Po, A.J. D Go, ACQUITY UPLC Ayss o E S Os (Prt 1). Wtrs Corporto, 2007: EN. Rrs 16. P. J. L, C. H. Po, A.J. D Go, ACQUITY UPLC Ayss o E S Os (Prt 2): Ov O Quty & Autrto. Wtrs Corporto, 2007: EN. 1. G. Kot, JAOCS. 2006, 83 (10): G. Kot, ASAE. 2001, 44 (2): ttp:// 4. ttp:// 5. H. Nour t. JAOCS. 1998, 75 (12): P.R.C. Nto t. JAOCS. 2004, 81 (12): Typ soy o ossts o 11% pt, 4% str, 24% o, 54% o, 7% o. Wtrs, ACQUITY UPLC, UPLC r rstr trrs o Wtrs Corporto. T S o Wt s Poss s trr o Wtrs Corporto. A otr trrs r t proprty o tr rsptv owrs Wtrs Corporto. Prou t U.S.A. Apr EN PDF Wtrs Corporto 34 Mp Strt Mor, MA U.S.A. T: F: