HPLC- ESI-MS HPLC-ESI-MS HPLC-ESI-MS HPLC 11 HPLC HPLC-ESI-MS. Asterias rollestoni Bell. LC- MS. Vol.11 No.1

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1 HPLC- ESI-MS * 200 Vol.11 No.1 ** HPLC-ESI-MS HPLC-ESI-MS HPLC HPLC-ESI-MS 11 HPLC - Asterias rollestoni Bell. [1~7] [1] [5~7] - - [8~] LC- MS * ** GY T32 jhchen@fio.org.cn

2 HPLC-MS 150mm 5μm 0.2 % A B 20uL 0.8mL/min HPLC-MS 260nm 60min time: min B%:5%-5%-10% HPLC -30%-40%-100%-100% Agilent DAD LC-MS XCT 6320 Agilent KQ-400KDE Milli- Q(18.2 MΩ) Millipore Z383K HERMLE THZ-8 20% 3 [10] Merck Milli-Q No g mL 20% mL 30min μm 3. HPLC-MS 1 Agilent Zorbax Bonus -RP C mm 250mm 5μm Diamonsil C mm V kPa N 2 12L/min V Scan m/z 50~1000 [10]

3 200 Vol.11 No.1 0 1h 0.5h 1 6 RSD RSD 0.86%~2.81% 0.41%~1.06% 2. HPLC 2 [1] RSD 20% RSD 2.62% ~4.5% C %~1.05% 3 C C 8 C h C 18 C 8 C 18 RSD 2.63% Zorbax Bonus-RP Diamonsil ~4.68% 0.7%~1.28% 48 h 1 C 18 C 18 B HPLC HPLC A % 0.1% A - 0.2% A HPLC-DAD HPLC-ESI-MS nm 260nm HPLC [11] [ 12] 3. HPLC 175

4 10 DAD C 10 H 12 N 4 O Time min HPLC Time min e abundance mau 2 15 HPLC-ESI-MS 40min (min) C 6 H 13 NO C 6 H 13 NO C H 11 NO C 5 H 4 N 4 O C H 12 N 2 O C 5 H 6 N 2 O C H 11 NO 2 C C 10 H 12 N 4 O 10 H 12 N 4 O C 5 H 4 N 4 O 12 [13] C C 10 H 12 N 4 O 10 H 12 N 4 O C 11 H 12 N 2 O 2 176

5 200 Vol.11 No ~ ~ B 2007 mau Time min HPLC No Similarity (Asterias rollestoni Bell). 17(1) 35~ C. 1(1) 1~3. 5 Sang-Seon Yun, Michael C. Thorndyke, Maurice R. Elphick. Identification of novel SALMFamide neuropeptides in the starfish Marthasterias glacialis. Comparative Biochemistry and Physiology, Part A, 2007, 147: 536~ Hai-Feng Tang, Yang-Hua Yi, Ling Li. Asterosaponins from the starfish Culcita novaeguineae and their bioactivities. Fitoterapia, 2005, 77: 28~34. 7 LI Guo-qiang, DENG Zhi-wei, LI Jun, et al. Chemical Constituents from Starfish Asterias rollestoni. Journal of Chinese Pharmaceutical Sciences, 2004, 13(2):81~ (LC/MS) ~40. Cai ZW, Lee FSC, Wang XR. A capsule review of recent studies on the application of mass spectrometry in the analysis of Chinese medicinal herbs. Journal of Mass Spectrometry, 2002, 37:l013~l RP-HPLC (1) 61~ (1) 73~ ~ HPLC (4) 380~381. Identification of active components in Asterias rollestoni Bell. by HPLC- ESI-MS and Study on Their HPLC Fingerprint Zhang Daolai, Chen Junhui, Wang Hong, Zhao Hengqiang, Cheng Hongyan QingDao Key Lab on Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of SOA, Qingdao, Wang Xiaoru 177

6 QingDao Key Lab on Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of SOA, Qingdao, Department of Chemistry and the Key Laboratory of Analytical Science of the MOE, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen , China Li Guoqiang School of Medicine and Pharmacy, Ocean University of China, Qingdao , China Objective: A new method based on high performance liquid chromatography - electrospray ionization mass spectrometry (HPLC-ESI-MS) was developed for the rapid identification of active compounds in Asterias rollestoni Bell and development of its fingerprints. Method: Samples were extracted by ultrasonic -assist extraction, and the extraction conditions were optimized. The developed HPLC -ESI -MS method was used to identification of the components in Asterias rollestoni Bell extract, and a chromatographic fingerprint based on HPLC analysis was established. Result: Eleven compounds in Asterias rollestoni Bell extract could be primary identified by ESI -MS on-line detection combined with literature review. The result of similarity evaluation for fingerprint indicated that the quality of different Asterias rollestoni Bell samples were not entirely consistent. Conclusion: This method has the advantages of simple operation, rapid measurement and it is a powerful tool for identification of active components in Asterias rollestoni Bell and its quality control. Keywords: HPLC-ESI-MS, Asterias rollestoni Bell, Fingerprint. (Continued from Page 167) Flash evaporation-gas chromatography-mass spectrometry for the analysis of volatile compounds in Ligusticum chuanxiong Hort. Zhang Cong Qi Meiling Fu Ruonong Department of Chemistry, School of Science, Beijing Institute of Technology, Beijing This paper describes a novel flash evaporation-gas chromatography-mass spectrometry (FE-GC-MS) for the analysis of volatile compounds in Ligusticum chuanxiong Hort. The results show that the optimum flash evaporation can be achieved by using ~4mg of the ground sample at 250 for 10s. In comparison with traditional steam distillation, the present FE-GC-MS method is rapid and only needs a few milligrams of the ground sample and a few seconds of flash evaporation time. It is an effective and feasible method for the quality control of traditional Chinese medicines (TCMs). Keywords: FE-GC-MS; volatile compounds; traditional Chinese medicines 178