V o l. 25 N o. 9 2 0 0 4 9 CH EM ICAL JOU RNAL O F CH IN ESE UN IV ERS IT IES 1632 1636,,,, (, 116011) H PL C2PAD 2M S,,.,. H PL C2PAD 2M S.,.,,. 2 ; ; O 652. 7 A 025120790 (2004) 0921632205,,., [1 5 ] [6, 7 ],. (TL C) [1 5 ] (H PL C) [5 7 ]. ( IMM CC) [8 ]. [9 ], [10 ]. TL C H PL C. 2 2 (H PL C2DAD 2M S) (R ad ices p aeon iae rubra) (L ig usticam w a llich ii)..,. 1 1.,.,.,.,,,,, [10 ].., F ig. 1 Flow chart of comprehen sive design in the research of com patibil ity : 2003208208. : ( : G19990554). : (1965 ),,,,,. E2m ail: liangxm @dicp. ac. cn
N o. 9 : 1633.,,,.,,,.,.,, 2 2 (H PL C2UV 2M S),,, ( ), ( ), ( ). 2 2. 1,. (C. P., ) ; (C. P. ) T ED IA ; M illiq ; 95% A. P. ( ). : 2150 g, 50 ml 95% 40 m in, 50 ml 40 ml 95% 1 h. 25 ml. : 2150 g, 50 ml 95% 40 m in, 50 ml 40 ml 95% 1 h. 25 ml.. 2. 2 : 5100 g, W aters A lliance 2690 ( 996 M illenn ium 32 ). : W aters Sph riso rb OD S1 (250 mm 210 mm, 5 Λm ). : (A ) 2110% (B ) ; A 5% ( ) 1 m in, 1 65 m in 50% ( ), 65 90 m in 100% ( ). 012 ml gm in; 5 ΛL, 10 ΛL. 2. 3 254 nm. F inn igan M A T T SQ, A PC I ;, 100 1 000; 400, 230, (N 2 ) 10 L gm in, (N 2 ) 4. 1 10 5 Pa. 3 3. 1 3. 1. 1, 2 2015% 2 2110% 2,, 2, 0 10 m in 10 80 m in, 40 50 m in, 4211 m in (R SD ) 4810% (n= 3). 2015% 2 2. 6, 7 8, 13 (R SD ) 3914% (n= 3), 015%, 13. 2110% 2,, (R SD ) 0 018%, (R SD ) 014% 612% (n= 3). 2 (A ). 2110%,,,,.
1 634 V o l. 25 2 (B ) (E). F ig. 2 The chromatogram s of blank sample (A), L igusticun wa llich ii (B), Rad ices p aeon iae rubra (C), com bined-decotion (D ) and co-decoction (E) 3. 1. 2,,.. 3, 10 ΛL. (R SD ) 0 018% (n= 3), (R SD ) 019% 612% (n= 3),.. 3,,., 1. 1,, R SD 011% 116% (n = 3), R SD 016% 1015%,. Table 1 The reproduc ibility of the method Peak Retention Peak Retention RSD (% ) Peak area RSD (% ) N o. tim egm in N o. tim egm in RSD (% ) Peak area RSD (% ) 1 3. 6 0. 10 399 756 2. 5 18 38. 0 1. 10 127 682 9. 4 2 4. 8 1. 60 149 485 8. 3 19 40. 6 0. 10 61 076 9. 7 3 6. 6 0. 00 169 393 6. 9 20 50. 6 0. 10 55 936 6. 0 4 14. 0 0. 00 41 270 8. 2 21 54. 4 0. 10 63 018 7. 4 5 16. 6 0. 60 44 388 10. 5 22 62. 8 0. 10 49 043 1. 2 6 19. 4 0. 70 108 130 5. 5 23 64. 4 0. 10 42 404 5. 1 7 20. 1 0. 40 234 197 3. 9 24 68. 1 0. 10 205 760 4. 3 8 21. 1 0. 20 51 510 4. 6 25 68. 7 0. 10 472 221 0. 6 9 22. 7 0. 50 90 374 8. 9 26 74. 6 0. 10 1 188 556 2. 4 10 23. 6 0. 70 41 365 9. 7 27 75. 5 0. 00 43 308 1. 8 11 26. 7 0. 20 453 004 4. 5 28 80. 3 0. 00 36 251 1. 4 12 30. 8 0. 10 89 763 7. 5 29 81. 9 0. 00 82 480 2. 0 13 31. 9 0. 26 230 814 10. 2 30 82. 2 0. 00 115 502 2. 1 14 33. 7 0. 20 48 201 5. 4 31 82. 6 0. 00 181 161 2. 3 15 34. 6 0. 20 45 327 8. 9 32 82. 8 0. 00 46 306 3. 1 16 35. 4 0. 10 46 151 7. 8 33 86. 6 0. 00 148 974 4. 1 17 36. 7 0. 10 120 011 6. 5 3. 2 3. 2. 1 ( 2), 5510 m in, ( 21 33) ; 3 55 m in, 1, 2, 3, 5, 7, 8, 9, 11, 12, 14, 15, 16, 17 20, 1, 2, 4, 6, 9, 12, 13, 15 17 33, 1, 2, 9, 12, 15, 17 20, 10,,. 3. 2. 2 W aters M illenn ium.
N o. 9 : 1635 33, 33.,,. 3 2015 m in, 1, 2, 3, 5 7, 4, 6 ; 2115 5510 m in 11, 14 17 20, 13, 18 19. 8, 9 10.,., 8, 9 10. 10 221, 263 325 nm, 10 224 264 nm, 10 233 325 nm. 5510 m in. 3. 2. 3,. 2., 1, 2, 3, 5, 7, 8, 9, 11, 12, 14, 15, 16 20, 4, 10, 13, 18 21 23. 6 17,.,. 1, 2, 3, 5, 7, 8, 9, 10, 11, 12, 15, 16, 17 20, 1, 2, 4, 9, 10, 12, 13, 14, 15, 17, 18, 19, 20 21 33, 1, 2, 9, 10, 12, 15, 17 20. 6,. Table 2 M olecular we ight of Rad ices p aeon iae rubra (RPR) and L igusticam wa llich ii (LW ), the ir co-decoction and combined-decoction 3 Peak N o. Co2decoction Com bined2 Com bined2 LW RPR Peak N o. Co2decoction decoction decoction LW RPR 1 342, 360 342, 360 360 342 18 224 224 224 2 376, 180 376, 180 180 376 19 224 224 224 480 3 170 170 170 20 584 584 584 4 181 181 181 21 208 208 208 5 446 446 446 22 204 204 204 6 23 204 204 204 7 496 496 496 24 192 192 192 8 446 446 267 446 25 194 194 194 9 526 526 354 526 26 382 382 382 10 167 167 167 27 380 380 380 11 480 480 480 28 380 380 380 12 526 526 526 29 380 380 380 13 194 194 194 30 380 380 380 14 446, 480 446, 480 446, 480 31 380 380 380 15 480 480 480 32 382 382 382 16 522 522 282 522 33 324 324 324 17 194 3 N o t to be determ ined. 3. 3 t2, 6, 10 17 (P < 0101),., 6 017 m in ( 3)., 6. 6 258 25618 nm. 6, 6. F ig. 3 Compar ison of co-decoction and com bined decoction
1 636 V o l. 25 [ 1 ] WAN G J ing2rong ( ), M A Zong2Yu ( ), YAN Yong2Q ing ( ) et al.. L ish izhen M edicine and M aterialm edica Research ( ) [J ], 2001, 11 (2) : 102 104 [ 2 ] WAN G X ian2yang ( ). Ch inese M edicine of Science and T echno logy ( ) [J ], 2002, 9 (3) : 161 162 [ 3 ] H E W ei( ), Q IN L in ( ), S I Shu2Yuan ( ). T raditional Ch inese M edicine ( ) [J ], 2002, 33 (7) : 600 602 [ 4 ] CH EN J ian2p ing ( ), TAN B ing2yan ( ), WU W ei2kang ( ) et al.. Ch inese Journal of Experim ental T raditionalm edical Fo rm ulae ( ) [J ], 2001, 7 (3) : 16 17 [ 5 ] ZHU D an2n i( ), YAN Yong2Q ing ( ), L I Zh i2m ing ( ). Ch ina Journal of Ch inese M aterial M edica ( ) [J ], 1998, 23 (8) : 483 485 [ 6 ] X IA Yun ( ), L I Zh i2m ing ( ), ZHU D an2n i( ). Ch ina Journal of Ch inese M aterial M edica ( ) [J ], 1998, 23 (4) : 230 232 [ 7 ] ZHU D an2n i( ), L I Zh i2m ing ( ), YAN Yong2Q ing ( ) et al.. Ch ina Journal of Ch inesem aterialm edica ( ) [J ], 1998, 23 (5) : 291 293 [ 8 ] L IAN G X in2m iao ( ). Ch inese Journal of Ch rom atography ( ) [J ], 1995, 13 (5) : 307 309 [ 9 ] LU Pei2Zhang ( ), ZHAN G Yu2Kui( ), L IAN G X in2m iao ( ). H igh Perfo rm ance L iquid Ch rom atography and It s Expert System ( ) [M ], Shenyang: L iaoning Publish ing House of Science and T echno logy, 1992: 181 [ 10 ] X IAO Hong2B in ( ), L IAN G X in2m iao ( ), LU Pei2Zhang ( ) et al.. Ch inese Science Bulletin ( ) [J ], 1999, 44 (6) : 588 596 M ethod for Chem ical Changes in Com patibility of Trad itional Ch inese M ed ic ine R ad ices P aeon iae R ubra and L itusticam W a llich ii L I X iu2l ing, X IAO Hong2B in, XU Q ing, W AN G L ong2x ing, L IAN G X in2m iao 3 (D alian Institu te of Chem ical P hy sics, Ch inese A cad em y of S ciences, D alian 116011, Ch ina) Abstract T he theo ry of herb compatib ility is essen tial part of traditional Ch inese m edicines (TCM ) p rescrip tion. N o w o rk has been repo rted on changes of m u ltip le componen ts in TCM compatib ility. It is the first tim e that basic idea abou t studying changes of m u ltip le componen ts in TCM compatility w as put fo rw ard. H igh2perfo rm ance liqu id ch rom atography2pho todiode array detecto r2m ass spectrom etry (H PL C2PAD 2M S) w as u sed in th is study. Info rm ation of reten tion tim e, u ltravio let (UV ) spectra and mo lecu lar w eigh ts w as compared to confirm the o rigin of peak s in TCM co2 decoction. T hen, changes of m u ltip le componen ts in TCM compatib ility w ere carried ou ṫ U n ifo rm ch rom atograph ic m ethod w as the foundation of basic idea. M eanw h ile, the o rigin s of peak s in TCM co2decoction w ere b reak th rough. To exp lo re the chem ical changes of compatib ility of R ad ices p aeon iae rubra and L itusticam w a llich ii, a rep roducib le and stab le ch rom atograph ic m ethod w as estab lished. T hen, ch rom atograph ic data w ere p rocessed w ith the un ifo rm ch rom atograph ic m ethod. Info rm ation of reten tion tim e, UV spectra and mo lecu lar w eigh t w as ob tained in H PL C2PAD 2M S run. By comparing reten tion tim e, UV spectra and mo lecu lar w eigh t of each peak in co2decoction w ith tho se of R ad ices p aeon iae rubra and L itusticam w a llich ii, the o rig in of each p eak in co 2decoct ion w a s confirm ed. F inally, the chem ical changes of compatib ility of R ad ices p aeon iae rubra and L itusticam w a llich ii in co2decoction w ere compared w ith tho se of com b ined2decoction. T he resu lts indicate that tw o peak s change in con ten t and one peak regenerate after compatib ility. Keywords H igh2perfo rm ance liqu id ch rom atography2pho todiode array detecto r2m ass spectrom etry (H PL C2PAD 2M S) ; Ch inese m edicine; H erb compatib ility (Ed. : A, G, X)