HPLC D eterm ina tion of ar istoloch ic ac ids in plan ts of A ristoloch ia L 1 by sta tic pressur ized l iqu id extraction

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1 364 Ch inese Traditional and Herbal D rugs HPLC 1, 1Ξ, 2, 1, 1 (11, ; 21, ) : g g,, g g,, :, , 120, 1013 M Pa, 10 m in, 40%, 1, 1100 gg g 4,,, ; : ; ; ; ; ; ; : R 28412; R : A : (2008) HPLC D eterm ina tion of ar istoloch ic ac ids in plan ts of A ristoloch ia L 1 by sta tic pressur ized l iqu id extraction L IAN G Q ing2you 1, ZH EN G Y ing 1, TAN G Ho i2yee 2, L I Shao2p ing 1, W AN G Y i2tao 1 (11 Institute of Ch inese M edical Sciences, U niversity of M acau, M acao, Ch ina; 21 Schoo l of H ealth Sciences, M acau Po lytechnic Institute, M acao, Ch ina) Abstract: Objective To op tim ize static p ressu rized liqu id ex traction (PL E) m ethod fo r the ex traction of aristo loch ic acids g and g (AA g and AA g ) from F ructus A ristoloch iae and study the influences of re2 lated facto rs1 M ethods T he un ivariate design w as in troduced1 T he operational param eters, such as the type of so lven t, particle size of the samp le pow der, ex traction temperatu re, p ressu re, static tim e, flu sh vo lum e, the num ber of cycles, and the amoun t of samp le w ere op tim ized1 Results T he op tim ized resu lt emp loyed m ethano l as ex traction so lven t, particle size of m eshes, ex traction temperatu re of 120, ex traction p ressu re of 1013 M Pa, static tim e of 10 m in, flu sh vo lum e of 40%, 1 cycle, and samp le amoun t of 1100 g1 T he m ethod w as app lied fo r fou r species of traditional Ch inese m edicinal m aterials in2 cluding F ructus A ristoloch iae, Cau lis A ristoloch iae M anshu riensis, R ad ix A ristoloch iae, and R ad ix A rsi2 toloch iae F ang ch i1 Conclusion T h is m ethod can be u sed to comp letely ex tract AA g and AA g from F ructus A ristoloch iae in once ex traction1 T he comparison show s that th is static PL E m ethod is better than u ltrason ication and Soxh let m ethods w ith h igher ex traction efficiency and less tim e2con sum ing1 It is also better than the dynam ic one in the ex traction of AA s from R ad ix A ristoloch iae1 Key words: F ructus A ristoloch iae; C au lis A ristoloch iae M anshu riensis; R ad ix A ristoloch iae; R ad ix A rsitoloch iae F ang ch i; aristo loch ic acid; static p ressu rized liqu id ex traction; H PL C A ristoloch ia con torta Bunge A 1 d ebilis Sieb1 et Zucc1,, [1 ], 3, , g ( A ) g ( B ), (aristo loch ic acids), [2, 3 ] [4 ], (aristo loch ic acid neph ropathy), TL C [5 ] L C2ES I2M S [6 ] UV [7 ] H PL C2DAD [8 ],, Ξ : : (049g2005gA 2R 1) : (1982 ),,, T el: Fax: E2am il: njlqy@ 1631com 3 T el: Fax: E2m ail: yzheng@um ac1mo

2 Ch inese Traditional and Herbal D rugs [1 ] [8 11 ] (p ressu rized liqu id ex traction, PL E), [12 ],,,,, g g, 1 A gilen t 1100,,, Chem station A SE200 (D ionex, Sunnyvale, ), Kn ifetec TM 1095 (Fo ss T ecato r Company, ) T ran son ic T I H 25 ( E lm a, ) 5415D ( Eppendo rf, Barkhau senw eg 1, H am bu rg, ) A 1 con torta Bunge A 1 d ebilis Sieb1 et Zucc1 A 1 m anshu riensis Kom 1 A 1 f ang ch i Y1C1 W u ex L 1D 1 Chou et S1M 1 Hw ang h,, g 27%, g 65%, M erck M illi Q P lu s (M illipo re, ) 2 Bedfo rd, 211 g g H PL C : Zo rbax SB C218 (250 mm 416 mm, 5 Λm ) (1215 mm 416 mm, 5 Λm ) ; 0101 mo lgl (A ) 2 (B ) ; : 0 24 m in, B % 30% ; m in, B % 30% 42% ; m in, B % 42 44%, 100%B 5 m in 10 ΛL ; [8 ] 254 nm ; : 110 ml gm in; 25 g g : 7123 m g, 10 ml, ( ΛggmL g, ΛggmL g ), - 20, g g 5, (SgN ) LOD (SgN = 3) LOQ (SgN = 10), 1 1 g g LOD LOQ Table 1 Regression equation, linear ity range, LOD and LOQ of AAg and AAg LOD r 2 g(λg ml - 1 ) gng LOQ gng g Y = X g Y = X :, g g 3, R SD < 115%, 9513% 10319% (n= 3) : g g, h 6, R SD 117%, g g 1 d g 3,, R SD < 2% (n= 3), 3 g g,,, 9414% 10014%, R SD 0145% 315% (n= 3), : 1100 g, 1 1,,, 1013 M Pa, 100, 5 m in, 40%, 1, ( mm ),,,, 25 ml, 0145 Λm : 2 (1 1) 2(1 1),

3 366 Ch inese Traditional and Herbal D rugs (1 1),, 2(n= 3) Table 2 Optim ization of extraction solven t (n= 3) g g(m g g - 1 ) g g(m g g - 1 ) (1 1) (1 1) : 3,, , (n= 3) Table 3 Optim ization of particle size (n= 3) g g g(m g g - 1 ) g g(m g g - 1 ) : 4, , 120 4(n= 3) Table 4 Optim ization of extraction temperature (n= 3) g g g(m g g - 1 ) g g(m g g - 1 ) : , 016 M Pa,, 1013M Pa 3, 5(n= 3) Table 5 Optim ization of extraction pressure (n= 3) gm Pa g g(m g g - 1 ) g g(m g g - 1 ) :, ( ),, 3 (P > 0105), (P < 0105),, :, ( mm ) 1100 g, 1013 M Pa, 120, 10 m in, 40%, : [13 ],, = A 1 n A i i= 1 100% A 1 (m g), i (), g g 95140% 97194% ( 6), g g :, g g, 6, ( ) 95%, 4 g g : [8 ] 1100 g, 50 ml, ml, 15 m in, 118 kw, ( rgm in, 5 m in), 0145 Λm : [10 ], 1100 g,, 80 ml 5 h, 100 ml, 0145 Λm

4 Ch inese Traditional and Herbal D rugs (n= 3) Table 6 PL E Recovery of Caulis A ristoloch iae M anshuriensis, Rad ix A ristoloch iae, Rad ix, A rsitoloch iae F angch i, and F ructus A ristoloch iae (n= 3) g% g g g g g g g g g g (n= 3) Table 7 D eterm ination of AAg and AAg in Caulis A ristoloch iae M anshuriensis, Rad ix A ristoloch iae, Rad ix A rsitoloch iae F angch i, and F ructus A ristoloch iae (n= 3) g g(m g g - 1 ) g g(m g g - 1 ) : 8, 3,,, 3 [14 ],,, 8 (n= 3) Table 8 Compar ison of extraction between PL E and traditional method (n= 3) gm in gh gml g g(m g g - 1 ) g ,,,,, [15 ],, 2 (1 1),,, ;, [15 ],,,,, (120 ) [16 ],,,,, O ng [16 ] g g m in,,,,, g g,

5 368 Ch inese Traditional and Herbal D rugs tgm in 12g 22g 12AA g 22AA g 1 (A) (B)(C) (D ) (E) HPLC F ig11 HPLC Chromatogram s of ar istoloch ic ac ids (A), F ructus A ristoloch iae (B), Caulis A ristoloch iae M anshuriensis (C), Rad ix A rsitoloch iae (D ), and Rad ix A rsitoloch iae F angch i (E) by pressur ized l iquid extraction,,,,,,,,, :,, : [ 1 ] [S ] [2 ],, 1 [J ]1, 2006, 26 (2) : [ 2 ] A rlt V M, Stibo rovam, Schm eiser H H 1 A risto loch ic acid as a p robable hum an cancer hazard in herbal rem edies: a review [J ]1 M utagenesis, 2002, 17 (4) : [ 4 ] V an H erw eghem J L, D ep ierreux M, T ielem ans C, et al1 Rap idly p rogressive interstitial renal fibro sis in young wom 2 en: association w ith slimm ing regim en including Chinese herbs [J ]1 L ancet, 1993, 341: [ 5 ] L o set J R, Raoelison G E, Ho stettm ann K1 A n L CgDAD 2 UV gm S m ethod fo r the rap id detection of aristo loch ic acid in p lant p reparations [J ]1 P lanta M ed, 2002, 68: [ 6 ] Chan S A, Chen M J, L iu T Y, et al1 D eterm ination of aris2 to loch ic acids in m edicinal p lant and herbal p roduct by liquid chrom atography2electro sp ray2ion trap m ass spectrom etry [J ]1 T alanta, 2003, 60: [ 7 ],,, 1 [J ]1, 2006, 12 (2) : [ 8 ] Zhang C Y, W ang X, ShangM Y, et al1 Sim ultaneous deter2 m ination of five aristo loch ic acids and two aristo lo lactam s in aristo lochia p lants by high2perfo rm ance liquid chrom atogra2 phy [J ]1 B iom ed Chrom atog r, 2006, 20: [9 ],,, 1 RP2H PL C A [J ]1, 2004, 29 (5) : [ 10 ],,, 1RP2H PL C A [J ]1, 2003, 23 (3) : [ 11 ],, 1 A 1[J ]1, 2001, 18 (2) : [ 12 ],,, 1 [J ]1, 2004, 29 (8) : [ 13 ] L i P, L i S P, L ao S C, et al1 Op tim ization of p ressurized liq2 uid extraction fo r Z2ligustilide, Z2butylidenephthalide and ferulic acid in A ngelica sinensis [J ] 1 J P harm B iom A nal, 2006, 401 [ 14 ] Zhao J, L i S P, Yang F Q, et al1 Sim ultaneous determ ination of saponins and fatty acids in Z iz ip hus jujuba (Suanzao ren) by h igh perfo rm ance liquid ch rom atography2evapo rative ligh t scattering detection and p ressurized liquid extraction [J ] 1 J Ch rom atog r A, 2006, 1108: [ 15 ] M ukhopadhyay S, L uth ria D L, Robbins R J1 Op tim ization of extraction p rocess fo r pheno lic acids from black coho sh (C im icif uga racem osa) by p ressurized liquid extraction [J ]1 J S ci F ood A g ric, 2006, 86: [ 16 ] O ng E S, W oo S O, Yong Y L 1 P ressurized liquid extraction of berberine and aristo loch ic acids in m edicinal p lants [J ]1 J Ch rom atog r A, 2000, 313: