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1 37 FENX I HUAXUE) ( Chinese Journal of Analytical Chem istry , 3 3 2, (, ) 2 (, ) 3 (, ), (DESI2MS), 2, DESI2MS, 5, 2, 1. 5 m in,,,,, 1 ( F ructus Evod iae),,, [ 1 ], [ 1, 2 ],,, [ 2 4 ] ( ),, 2,, [ 5 ] LC2MS,,, ( ESI) (APC I) (DESI) [ 6 8 ],, ( ), DESI, DESI 2004, [ 9, 10 ] [ 11 ] [ 12 ] [ 13 ] [ 14 ] [ 15 ] DESI2MS, DESI2MS [ 12 ], LTQ ( ) ; (DESI) ( ) ; ( ) ( ) ;, ( ) ;, ; (No ) 3 E2mail: zhjianhb@ gmail. com

2 ( D ES I) DESI ( ESI),, 32D, ESI LTQ, DESI [ ] (C ID ), 1. 5, 20% 30% g, mm,,, DESI, 1 mm,, DESI, 1. 5 m in D ES I2M S Th; 0 ml /m in; 3 ml /m in; 300 m / s; 5 kv, 12 V, 100 V; 275 ; = (V /V ) ; 5 mm; 2 mm; ( ) 45 ; ( ) , (Datura stramonium ) DESI2MS, 1 a 1a, DESI [ 11 ],, (m / z 304) C ID, 1b, [ 11 ] DESI ( ), 1 DESI2MS ( a) ( b) Fig. 1 Desorp tion electrosp ray ionization (DESI) 2MS of Datura stramonium ( a) and C ID spectrum of p rotonated scopolam ine (m / z 304) ( b), showing rep roducibility and app rop riate operation parameters for DESI experiments , 72 (32tygloyloxy26, 72dihydroxytropane) ; 2. ( scopolam ine) ; 3. 3, ( 3, 62ditygloyloxy27 2hydroxytropane) ; ( 32acetoxy262hydroxytropane) ; (3 2tygloyloxy262isovaleroyloxy272hydroxytropane) ; (32tropoyloxy262tygloyloxytropane) DESI, 2 [ 6 ], 1% 1%,

1 Desorp tion electrosp ray ionization (DESI) 2MS of Datura stramonium ( a) and C ID spectrum of p rotonated scopolam ine (m / z 304) ( b), showing rep roducibility and app rop riate operation

3 2 : ( 1 1, V /V ) 2 2 ( , V /V ) 2 2 ( , V /V ),,,,, DESI,, DESI 2 [ 6, 13 ],,,,, 2 2 ( , V /V ) DESI 2 2 ( , V /V ), 3 L /m in, 3 L /m in 3. 2 D ES I,, DESI2MS 2 2, DESI2MS, m / z (S /N 3), [ 5, 16, 17 ], ( 303) ( 307) ( 319) ( 287) ( 305),,,, DESI2MS 2, m / z , 5,,, C ID 3a 3b 2 DESI2MS Fig. 2 DESI2MS of F ructus Evodiae p lant tissue using acidic sp raying solvent 3 C ID Fig. 3 DESI2MS/MS of evodiam ine and evodiam ide in p lant 3a m / z 171 C 8 H 7 NO ( ), C 11 H 10 N 2 ( ) m / z 134; m / z 134 m / z 171,, 3b, m / z 178 C 9 H 8 N ( ),,, CH 3 H 2 m / z 161, CH 3 NHCH 2 m / z 134 m / z 134,, m / z 320 m / z 304, 144, C 9 H 8 N 2 O 2 ( ) ; m / z 288, m / z 270; m / z 306 m / z 288, H 2 O, 5, [ 5, 16, 17 ], DESI2MS m / z 304, 308, 320, ( 303) ( 307) ( 319) ( 287) ( 305) C ID [ 5 ] : tissue

2 DESI2MS of F ructus Evodiae p lant tissue using acidic sp raying solvent 3 C ID Fig.

4 , ( Na + ), DESI2MS m / z 330, 637 ( 307 ) (M + Na + ) ( 2M + Na + ) ; m / z 326, 629 ( 303) DESI, [ 13, 15 ], LC2ESI2MS [ 5 ] 3. 3 DESI, DESI2MS, DESI 2 (m / z 126) [ 12 ],,,,,,,,,,, [ 5 ], [ 5 ], DESI,, [ 12 ] [ 13 ],, 2, DESI,, DESI2MS, m / z 304, m / z 304 ( 1 3),,, DESI2MS,, DESI2MS ( PCA ), References 1 Pharmacopoeia Comm ission of the M inistry of Public Health, P. R. China ( ). A Coloured atlas of the Chinese M ateria M edica Specified in Pharm acopoeia of the People s Republic of China ( ). Guangzhou ( ) : Guangdong Science and Technology Press( ), Zhao Dong2Mei( ), Zhang Ying ( ), B i Kai2Shun ( ). Chinese J. Pharm. A nal. ( ), 1999, 19: L iu Yan2W en ( ), Chen Shu2He ( ), Lu Xi2Zhen ( ), Xia Xi ( ), Ye Cong2J in ( ). Chinese J. Hospital Pharm. ( ), 1996, 16: L i Q in2yun ( ), Hong Xiao2Kun ( ), W ang Zhi2Hua ( ), W ei Hong ( ), W ang Zhi2W ei ( ). Chinese J. pharm. A nal. ( ), 2000, 20: Zhang Xue2Q in ( ), Zhou Xin ( ), W ang Dao2Ping ( ), Hao Xiao2J iang ( ). Chinese J. A nal. Chem. ( ), 2005, 33 (2) : Takats Z, W iseman J M, Cooks R G. J. M ass Spectrom., 2005, 40:

ission of the M inistry of Public Health, P. R. China ( ). A Coloured atlas of the Chinese M ateria M edica Specified in Pharm acopoeia of the People s Republic of China ( ).

5 2 : L i J ian2q iang( ), Zhou Yu2Fen ( ), D ing J ian2hua ( ), Yang Shui2Ping( ), Chen Huan2W en ( ). Chinese J. A nal. Chem. ( ), 2008, 36 (9) : Takats Z, W iseman J M, Gologan B, Cooks R G. Science, 2004, 306: Zhou Yue2M ing( ), J in W ei( ), Chen Huan2W en ( ), Xu Rui2Feng ( ). Chinese J. A nal. Chem. ( ), 2007, 35 (4) : Takats Z, Cotte2Rodriguez I, Talaty N, Chen H W, Cooks R G. Chem. Comm un., 2005: W iseman J M, Ifa D R, Song Q, Cooks R G. A ngew. Chem. Int. Ed., 2006, 45: Talaty N, Takats Z, Cooks R G. A nalyst, 2005, 130: Chen H W, Talaty N, Takats Z, Cooks R G. A nal. Chem., 2005, 77: Chen Huan2W en ( ), Zhang Xie ( ), Luo M ing2b iao ( ). Chinese J. A nal. Chem. ( ), 2006, 34 (4) : Chen Huan2W en ( ), L im ing( ), Zhou J ian2guang ( ), Fei Q iang ( ), J iang J ie ( ), Zhang Tian2Mu ( ), Zhang Xie ( ), J in Q in2han ( ). Chem. J. Chinese U niversities ( ), 2006, 27: Tang Yuan2Q ing ( ), W u Ke2Mei ( ), Feng Xiao2Zhang ( ), Huang L iang ( ). A cta Pharm. S inica. ( ), 1998, 33: Tang Y Q, Feng X Z, Huang L. J. Chinese Pharm. Sci., 1997, 6: D esorption Electrospray Ion iza tion M a ss Spectrom etry for Fa st D etection of A lka lo ids in F ructus Evodiae CHEN Huan2W en 1, 3, ZHENG J ian 3 2, 3, WANG W ei2ping 1, CHEN Chang2L in 1, WANG Zhi2Chang 1 1 ( East China Institute of Technology, Fuzhou 34400) 2 (B eijing Centre for Physical and Chem ical A nalysis, B eijing ) 3 (College of Chem istry, J ilin U niversity, Changchun ) Abstract Desorp tion electrosp ray ionization mass spectrometry (DESI2MS) was emp loyed for fast direct de2 tection of 5 alkaloids such as evodiam ide, evodiam ine, hydroxyvodiam ine, rutae carp ine and goshuyuam ide2 p resented in F ructus Evod iae herb p lant. The operation parameters for both DESI and LTQ instrument were op2 tim ized and tested by p reviously exam ined p lant tissue of Datura Stramonium so that a reliable fingerp rint of the F ructus Evod iae tissue was generated successfully using a m ixture of methanol/water/form ic acid ( ) as electrosp ray liquid. The alkaloids detected gave p redom inant signals at m / z 308, 304, 320, 288 and m / z 306, which were corresponding to the p rotonated molecules of evodiam ide, evodiam ine, hydroxyvodia2 m ine, rutae carp ine and goshuyuam ide2, respectively. The structures of the p rotonated molecules were con2 firmed w ith high confidence by tandem DESI2M S/M S, which was facilitated by the unique features of LTQ mass spectrometer. Ionic adducts of alkaloids and sodium were also commonly observed in DESI mass spectra of the p lant tissue, and possible interference caused by dust, fake tissues were also investigated experim ental2 ly. A single run was comp leted in 1. 5 m in, p roviding a fast method for fingerp rinting volatile compounds in p lant tissue. It has been demonstrated that DESI is not only potentially useful for the quality monitoring of p roducts in pharmaceutical p rocesses, but also useful to discrim inate authentic or fake F ructus Evod iae based on their mass spectral fingerp rints. Keywords Desorp tion electrosp ray ionization, mass spectrometry, F ructus Evodiae, fast direct detection (Received 26 March 2008; accep ted 24 November 2008)

Chem. ( ), 2007, 35 (4) : 621 10 Takats Z, Cotte2Rodriguez I, Talaty N, Chen H W, Cooks R G. Chem. Comm un., 2005: 1950 1952 11 W iseman J M, Ifa D R, Song Q, Cooks R G. A ngew. Chem. Int. Ed.

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