Analysis of Volatile Compounds from B u pleur um by Static Headspace2Gas Chromatography2Mass Spectrometry

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Mitchell Strickland
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1 Journal of Chinese Mass Spectrometry Society Vol. 26 No. Aug , 1, 1,, 2 (1.,, ; 2., ) : 22 6,, % 60 :, 25 %44 % ; 8. 1 %17. % ; 10. %7. 0 % ( RSD) % % : 2 2 (SH2GC/ MS) ; ; ; :O ; R28411 :A : (2005) Analysis of Volatile Compounds from B u pleur um by Static Headspace2Gas Chromatography2Mass Spectrometry L IAO Yuan2xi 1,WAN G Hao2yang 1, GUO Yin2long 1,,SHAO Ying2nan 2 (1. S hanghai M ass S pect roscop y Cent re, S hanghai I nstitute of Organic Chemist ry, Chinese A cadem y of Sciences, S hanghai 20002, China; 2. L uoy ang Minsheng Pharmaceutical Com pany w ith L imited L iabilit y, L uoy ang , China) Abstract : A static headspace2gas chromatograp hy2mass spectrometry ( SH2GC/ MS) met hod was used to analysis volatile compounds f rom the six kinds of B u pleurum f rom different ar2 eas. The approach of mass spectrogram searching combining wit h retentive index comparing was used to identify compounds. Sixty compounds whose percentage is more than 0. 2 % were identified f rom six medicines. The main compounds of t hese essences were acyclic al2 dehyde (25 %244 %), terpene (8. 1 %217. %) and terpene derivatives ( 10. %27. 1 %). The relative standard derivation (RSD) of t his method was in t he range of % %. The met hod is usef ul in analyzing volatile compounds f rom Chinese Traditional Medicine. Key words : static headspace2gas chro matograp hy2mass spect ro met ry ( S H2GC/ MS) ; reten2 tive index ; B u pleurum ; volatile compound : ; : : ( ) :(1981),( ),,,E2mail : sioc. ac. cn :(196),( ),,,E2mail : sioc. ac. cn

2 188 26, ( ) B u pleurum Chi nese DC. ( ) B. S corz oneri f oli um Willd., [1 ], [2 ], 70 ev ;150 ; [ ] ; [4 ] 2 ; [ 5 ] 2 2 ; [6 ] ,,,,, 2 2 [7 ] 2 2, [ 810 ] CP2800 Sat urn 2000 :(Varian) ;Sat2 urn GC/ MS Workstation ( Version 5. 52) COMBI PAL ( ) PAL System 112 : ; ( C62C44 ) : Chem. Service 11 GC/ MS : HP25MS ( 5 % 95 % ) ( 0 m mm 0. 25m) ;; 250 ; : 0, 2 min, / min min ; min ; : 1 ml/ min, ( EI) ; m/ z Saturn N IST g 10 ml, min,50 r/ min 00L GC/ MS 2 211, [11 ], NaCl,,, NaCl, 5 % 10 % 20 %,10 %,10 %,,,, 212 6,0 min, 1 :120 6, 120 [ 9 ] 0 min,,

3 : [9 ] 1 Fig. 1 Influence of headspace heating temperature on peak area of volatile compounds 1 2 ( 2pinene) ;2 ( hinesol) ; 2 ( 2eudesmol) ; 4 ( heptanal) ; 5 22 (22pentyl2furan) ;6 (hexanal) 21 6 : %( ) % () % (22 ). 9 %() % ( 2 ) % ( 2 ) 214, [10 ] 2 2, , 2 99, 2 982,, (1) N n, N n 1, t, tn < t < t N R I = 100 n ( N2n) ( t2t n) / ( t N2t n) (1) (1) % ( a) 2 ( b) Fig. 2 Mass spectra of 2pinene( a) and 2pinene( b),, 25 % 44 %, 8. 1 %17. %, % 7. 0 %,6, GC/ MS Fig. TIC of volatile oil from B. Scorzoneri f olium Willd. by static headspace2gc/ MS

4 Table 1 Volatile compound in the headspace of the sample No1 Compound Mr / % 1 2 2methyl2butanal methyl2butanal pentanal pentanol propyl2furan hexanone hexanal furfural met hyl212pentanol n2butyl2furan heptanal thujene pinene camp hene (12)2 [ ] methylene212(12methylethyl)2bicyclo [ ]oct212ene 16 benzaldehyde methyl2furfural pinene octen22ol met hyl22octanone pentyl2furan phellandrene octanal p2cymene phellandrene ,22ethyl222methyl21,2hexadiene benzeneacetaldehyde dimethylstyrene met hyl benzoate undecane nonanal methyl22cyclohexene212carboxaldehyde ,6221,,5,722,62dimethyl21,,5,72octatet raene hydroxyhomoadamantane (12 ) methoxy242methyl222(12met hylethyl)2benzene (12 ) methoxy242methyl212(12met hylethyl)2benzene

5 : No1 Compound Mr / % 7 anethole isobronyl acetate tetradecane [ (52 222) ] [ (52methyl222furanyl) methyl ]222furancarboxaldehyde 41 4,5,6,72[c ]4,5,6,72tetramet hylp hthalide isobornyl p ropionate cyperene butyl212octanol gurjunene cedrene caryophyllene , ,42dimethoxy222methyl252isopropyl2benzene 49 thymohydroquinone dimet hyl et her elemene gurjunene D germacrene D curcumene hexyl212octanol cuparene hexadecane hinesol eudesmol heptadecane methyl2hexadecane :,2 6, /,2 g,, 2 2 : [1 ]. ( ) [ S]. :, [2 ]. [ M ]. :, [ ],. 2 [J ]., 200,22 (1) : [4 ],,,.. / [J ].,1996, 15 (5) : 811. [5 ]. [J ]., 1994, 9 (1) : 9698.

6 [6 ],. [J ]., 1991, 21 (1) : [7 ],,,. 2 2 [J ]., 2004, 10 () : [8 ],,,. [ J ]., 1995, 15 (4) : 120. [9 ] Zelda P. Optimization of Conditions in Static H2 eadspace GC [ J ]. J High Resolut Chromatogr, 1992, 15 (12) : [10 ] Gonzalez FR, Nardillo AM. Retention Index T2 emperature2programmed Gas Chromatography [J ]. J Chromatogr A,1999, 842 : [11 ],,,. 2 2 [J ]., 2004, 2 (1) : (CN : / R, ISSN : ) : 195,,,,,,;,, 1999,2001 ( ) ;2002, ,,A4 15, 180 :22 2, :M105,, :1, : : : , : , ac. cn (http :/ / www. netshow. com. cn ) 2001,,,, ,,,,;,; 100,,,,! :http :/ / promotion. instrument. com. cn,,,,, : E2mail com. cn :

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