25 3 2004 8 Journal of Ch inese M ass Spectrom etry Society V o l. 25 N o. 3 A ug. 2004 -, 3, (, 710061) : 2 (GCgM S), N IST GCgM S,, : 22, 16, : ; ; 2 (GCgM S); : O 657. 63; Q 949. 763. 3 : A : 100422997 (2004) 032150205 Ana lysis of the Com ponen t and F ingerpr in t of Effective Part of L igusticum Chuanx iong Horṫ by Ga s Chroma tography-m a ss Spectrom etry L IAN G M ing2jin, H E L ang2chong 3,L I Yong2m ao (Colleg e of P harm acy, X i, an J iaotong U niversity, X i, an 710061, Ch ina) Abstract: T he com ponen ts of lipoph ilic part of L igu sticum Chuanx iong Ho rṫ (L CH ) w ere analyzed by u se of gas ch rom atographygm ass spectrom eter (GCgM S) w ith N IST lib rary. U nder the ch rom atograph ic condition s, the sam p les of L CH from differen t p lace w ith differen t batch w ere m easu red and the comm on peak s in the fingerp rin t w ere confirm ed. Tw en ty tw o com pounds in lipoph ilic part of L CH w ere iden tified and six teen of them w ill be u sed as comm on peak s of the fingerp rin t to con tro l the quality of L CH. T he fingerp rin t w ith active com pounds can basically illu strate the com po sing character of lipoph ilic part of L CH and the quality of L CH can be con tro lled by th is m ethod. Key words: m a ss sp ect rom et ry; study on L igu st icum Chuanx iong Ho rṫ ; ga s ch rom atography2m ass spectrom etry (GCgM S) ; effective part; fingerp rin t : 2003212210; : 2004203226 : : (20075020) : (1975 ), ( ),,, E2m ail: L iangm j@m ailsṫ xjtu. edu. cn 3 : (1957 ), ( ),,, E2m ail: helc@m ailsṫ xjtu. edu. cn
3 : 2 151 (R h izom a Chuanx iong) (E I) 200 ; L igu sticum chuanx iong Ho rṫ, (T IC) ; 1. 0 ΛL, 1. 2 ml gm in; [ 1, ], 2. 5 m in, AD P 114, 1. 4. 1 [ 2 4 ] [ 5 7 ] 20. 1 m g, 50 ml, 1 ml 0. 402 m g, 1. 4. 2,, 20, 0. 5 kg, 1 L CO 2 [ 8 10 ],, GCgM S,, [ 11 13 ] 20. 0 M Pa, 40, 40, kggh 3 h,,, 18. 6 g, GCgM S, 3. 72% 40 m g, 10 ml,,,, 1 111 1. 4. 3 GCgM S GCgM S2Q P2010 2 : 1. 0 ΛL, 1. 3. 1 Sh im adzu, GCgM S so lu tion, GCgM S N IST ; DB 25M S ( : 30 m 0. 25 mm, 0. 25 Λm, 1),, A gilen t ( ) ; HA 220250206 (Αi), : (A i% ) 115 112 1. 5. 1 ( : 20021102) : M eker ;, 1. 0 ΛL GCgM S :, GCgM S, 6 0. 5% 16 (Αi) R SD ( : 0. 1% 20011207 20021006 20021102), 1. 5. 2 ( : 20021102) 6, 1. 0 ΛL GCg (L igu sticum Chuanx iong Ho rṫ ) ; M S, 16 (L igu stilide) :, (Αi) R SD 0. 1% (H PL C) > 98% 113 1. 3. 1 DB 25M S ( 30 m 0. 25 mm, 0. 25 Λm ),, 16 Αi R SD : 80, 2 m in, 10 gm in 250, 11 m in; 1. 5. 3 ( : 20021102) 1, 0 2 6 12 24 48 h 1. 0 ΛL GCgM S, 0. 1% 116 1. 3. 2 250 ; 1. 6. 1, 12 : ; 50; 250 ;,
152 25 a (L igustilide) ; b (effective part of L CH ) GCgM S, Αi A i%,,,, GCgM S 1,,, [ 14 16 ],,, 1 (a), GCgM S (b) GCgM S, F ig. 1 Chromatogram s of L igustilide (a) and effective part of LCH (b) by GCgM S,, 212 [ 5 7 ] 1. 6. 2 CO 2,, 0. 5%, Αi A i% 9 CO 2 (80% ), ( 0. 1% ) 16, CO 2 0. 758 1. 323, 12 ( 16 98% ), GCgM S, tr 14. 402 m in, 16 2,,, (m gz, % ) : 190 (M +, 66. 3) 161 (M + 2C 2H 5, 95. 4) 148 (M + 2C 3H 6, 94. 9) 133 (M + 2C 3H 5O, 24. 1) 105 (M + 2C 4H 6O 2, 76. 5) 77 (M + 2C 6H 9O 2, 2 46. 5) N IST [ 17, 18 211 ] CO 2,,,,,,,, (40 ),, 213, GCgM S GCgM S,,
3 : 2 153 16, 0. 758 16 GCgM S 1. 323, (R SD % ) < 0. 1%,, 16,, 12 1 Table 1 Analytical result of the com ponen ts in effective part of LCH gd a N o. compound trgm in mo lecular mo lecular fo rm ula w eigh t 1 dim ethyl phthalate 10. 928 C10H 10O 4 194 2 eudesm a24 (14), 112diene 11. 574 C15H 24 204 3 3, 52 3, 52ditertbutyl2pheno l 11. 635 C15H 24 204 4 diethyl phthalate 12. 655 C12H 14O 4 222 5 decane 12. 767 C14H 30 198 6 12(2, 42 ) 212 [ 12(2, 42dim ethylphenyl) 2 12p ropanone ] 13. 491 C11H 14O 162 7 butylidene phthalide 13. 730 C12H 12O 2 188 8 62 21, 42 62butyl21, 42cyclohep tadiene 13. 959 C11H 18 150 9 Α2 Α2butyl2benzenem ethano l 14. 221 C11H 16O 164 10 42 222 42m ethyl222pyridinam ine 14. 328 C6H 8N 2 108 11 ligustilide 14. 413 C12H 14O 2 190 12 5, 7, 82 5, 7, 82trim ethyl2dihydrocoum arin 15. 111 C12H 14O 2 190 13 tetradecano ic acid 15. 636 C14H 28O 2 228 14 dibutyl phthalate 15. 703 C16H 22O 4 278 15 palm itic m ethyl ester 16. 345 C17H 34O 2 270 16 hep tadecano ic acid 16. 677 C17H 34O 2 270 17 hexadecano ic ethyl ester 17. 028 C18H 36O 2 284 18 9, 122 9, 122octadecadieno ic acid m ethyl ester 18. 008 C19H 34O 2 294 19 92 92octadecadieno ic acid m ethyl ester 18. 069 C19H 36O 2 296 20 9, 122 9, 122octadecadieno ic acid 18. 348 C18H 32O 2 280 21 92 92octadecadieno ic acid 18. 400 C18H 34O 2 282 22 octadecano ic acid 18. 626 C18H 36O 2 284 2 GCgM S F ig. 2 M ass spectrum of L igustilide by GCgM S : [1 ] [S ]. 2000 ( ): 37. [2 ],,,. [J ]., 1999, 15 (3): 281 282. [ 3 ] L im in, Shunno suke H anda, Yasuo Ikeda, et al. Specific Inh ib iting Characteristics of T etram ethylpyrazine, O ne of the A ctive Ingredien ts of the Ch inese H erbal M edicine Chuanxiong on P latelet T h rom bus Fo rm ation U nder H igh Shear R ates [ J ]. T h rom bo sis R esearch, 2001, 104 : 15 28. [4 ] T saia Ch inchuan, L ai T ungyuan, H uang W eichan, et al. Inh ib ito ry Effects of Po tassium Channel B lockers on T etram ethylpyrazine2induced R elaxation of R at A o rtic Strip in V itro [J ]. L ife
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