HPLC- ESI-MS * 200 Vol.11 No.1 ** 266061 266061 361005 266003 - HPLC-ESI-MS HPLC-ESI-MS HPLC HPLC-ESI-MS 11 HPLC - Asterias rollestoni Bell. [1~7] [1] [5~7] - - [8~] LC- MS * ** 173 2008-11-04 200-01-06 08 08-02-05-04 GY-022008T32 E-mail: jhchen@fio.org.cn
HPLC-MS 150mm 5μm 0.2 % A B 20uL 0.8mL/min HPLC-MS 260nm 60min time:0-10-20-30-40-50-60min B%:5%-5%-10% HPLC -30%-40%-100%-100% 1. 1 10 1. 1 2 1100 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 1 10 2. No. 1 2008.03.05 40 2 2008.03.07 2.0g 3 2008.04.02 100mL 20%4 2008.04.05 50mL 30min 5 2008.04.16 0.45μm 3. HPLC-MS 1 Agilent Zorbax Bonus -RP C 18 4.6mm 250mm 5μm Diamonsil C 18 4.6mm 2 4500V 310.27kPa N 2 12L/min 350 100V Scan m/z 50~1000 [10] 6 6 2008.05.07 7 2008.05.12 8 2008.05.25 2008.06.13 10 2008.06.28 174
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 18 0.73%~1.05% 3 C 18 0 1 3 6 C 8 C 18 12 24 48h 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 4. 0.2% 0.1% A - 0.2% A HPLC-DAD HPLC-ESI-MS 1 1 260nm 260nm HPLC [11] [ 12] 3. HPLC 175
10 DAD 3 2 10 2 1 2 3 10 7 3 1 C 10 H 12 N 4 O 5 11 2 10 7 10 4 5 6 11 15 2 7 8 12 13 14 1 10 7 5. 10 20 30 40 10 Time min 2 80 5 6 2 60 HPLC 10 10 40 4 11 7 2 20 1 3 8 12 13 14 15 10 0 10 20 30 40 Time min e 1 1 2 10 abundance mau 2 15 HPLC-ESI-MS 40min (min) 15 15 1 8.28 131 C 6 H 13 NO 2 2 8.82 131 C 6 H 13 NO 2 3 11.04 181 C H 11 NO 3 4 12.82 136 C 5 H 4 N 4 O 12 5 13.54 244 C H 12 N 2 O 6 12 6 15.44 153-7 17.32 126 C 5 H 6 N 2 O 2-8 18.61 - - - - 1.63 165 C H 11 NO 2 C 10 22.76 268 C 10 H 12 N 4 O 10 H 12 N 4 O 5 5 11 24.60 283 - - 12 25.63 136 C 5 H 4 N 4 O 12 [13] C 13 27.4 268 C 10 H 12 N 4 O 10 H 12 N 4 O 5 5 14 2.2 - - - - 15 32.05 204 C 11 H 12 N 2 O 2 176
200 Vol.11 No.1 4 6 0.80 7 0.0 1 2003 17~1. 1.. 2. 3. 2000 18 2 56~60. 3. 2005 4 B 2007 mau 100 80 60 40 20 0 10 20 30 40 Time min 2 3 10 HPLC No. 1 2 3 4 5 6 7 8 10 Similarity 0.4 0.67 0.4 0.76 0.3 0.65 0.6 0.2 0. 0.8 (Asterias rollestoni Bell). 17(1) 35~37.. - 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: 536~542. 6 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):81~86. 8. (LC/MS). - 2005 7 5 33~40. 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~l024. 10.RP-HPLC. 2005 21(1) 61~63. 11.. 2005 23(1) 73~75. 12. -. 2007 7 5 113~121. 13. HPLC. 2004 2(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, 266061 Wang Xiaoru 177
QingDao Key Lab on Analytical Technology Development and Standardization of Chinese Medicines, First Institute Oceanography of SOA, Qingdao, 266061 Department of Chemistry and the Key Laboratory of Analytical Science of the MOE, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China Li Guoqiang School of Medicine and Pharmacy, Ocean University of China, Qingdao 266063, 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 100081 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