Rapid Analysis Alkaloids in Lotus Seeds by Extractive Electrospray Ionization Mass Spectrometry†

doi:10.7503/cjcu20131121

Abstract

Abstract:

To identify alkaloids in lotus seeds rapidly and to distinguish fresh and aged lotus seeds, using self-developed extractive electrospray ionization source, ethanol extracts of lotus seeds were directly analyzed by mass spectrometry without any sample pretreatment. The MS were further analyzed using principal component analysis(PCA). The results showed that optimum conditions of ionization voltage, capillary temperature and sample flow rate were 3.5 kV, 250 ℃, and 5 μL/min, respectively. Liensinine, neferine, lotusine, nucife-rine and O-demethylation nuciferine were found in the ethanol extracts by tandem mass spectrometry, of which signal intensities showed special change trends. Lotus seeds of different storage time and aging degree were clearly distinguishable from each other by PCA. This method is of high sensitivity and high analytical speed, without complex sample pretreatment. The method in this paper is fast and effective to identify alkaloids in real samples with complicated matrix, and combined with chemometrics, it is also used to distinguish fresh and aged lotus seeds.

Key words: Extractive electrospray ionization mass spectrometry, Lotus seed, Principal component analysis, Alkaloid

CLC Number:

O657

TrendMD:

FANG Feifei, DU Shangguang, DAI Ximo, GUO Xiali, CHEN Huanwen, LUO Liping. Rapid Analysis Alkaloids in Lotus Seeds by Extractive Electrospray Ionization Mass Spectrometry^†[J]. Chem. J. Chinese Universities, 2014, 35(4): 730.

Figures/Tables 8

Fig.1 Effect of ionization voltage on the signal intensity of m/z 625

Fig.2 Effect of ion tube temperature on the signal intensity of m/z 625

Fig.3 Effect of sample injected speed on the signal intensity of m/z 625

Fig.4 Total ion chromatogram (TIC)(A) and selected ion diagrams of m/z 611(B), m/z 625(C), m/z 314(D), m/z 282(E) and m/z 296(F)

Fig.5 MS/MS spectra(A—E) of five alkaloids in ethanol extract of lotus seeds(A) Liensinine m/z 611; (B) neferine m/z 625; (C) lotusine m/z 314; (D) O-demethylation m/z 282; (E) nuciferine m/z 296.

Fig.6 Structures of five alkaloids in ethanol extract of lotus seeds(A) Liensinine m/z 611; (B) neferine m/z 625; (C) lotusine m/z 314; (D) O-demethylation m/z 282; (E) nuciferine m/z 296.

Fig.7 Signal intensity changes of five alkaloids in the ethanol extracts from lotus seeds with different storage time

Fig.8 2D plot of PCA score results for the ethanol extract from lotus seeds with different storage time by EESI-MS(A), loading 1 vs. loading 2 plot(B), 2D plot of PCA score results for m/z 611, 625, 314, 282 and 296(C) and loading 1 vs. loading 2 plot(D)

References 15

[1]	Wang J. L., Hu X. M., Yin W. H., Cai H. S., Journal of Chinese Medicinal Materials,1991, 14(6), 36—38
	(王嘉陵, 胡学民, 尹武华, 蔡鸿生. 中药材, 1991, 14(6), 36—38)
[2]	Luo X. B., Chen B., Liu J. J., Yao S. Z., Anal. Chim. Acta,2005, 538(1), 129—133
[3]	Chen W. Z., Ling X. Z., Ding G. S., Acta Pharmaceutica Sinica,1962, 9, 277—279
	(陈维洲, 凌秀珍, 丁光生. 药学学报, 1962, 9, 277—279)
[4]	Pan Y., Cai B. C., Yang G. M., Cao L., Shen A. Q., Journal of Nanjing University of Traditional Chinese Medicine,2005, 21(4), 243—244
	(潘扬, 蔡宝昌, 杨光明, 曹亮, 沈爱琴. 南京中医药大学学报, 2005, 21(4), 243—244)
[5]	Wu S. H., Sun C. R., Cao X. J., Zhou H., Hong Z., Pan Y. J., J. Chromatogr. A,2004, 1041(1), 153—162
[6]	Luo L. P., Zhao Z. F., Dai X. M., Zhang X., Liu Y. L., Zhang X. L., Zhang W. J., Ouyang Y. Z., Trans. Chin. Soc. Agri. Engi., 2013, 29(7), 261—266
	(罗丽萍, 赵占锋, 戴喜末, 张茜, 刘亚丽, 张兴磊, 章文军, 欧阳永中. 农业工程学报, 2013, 29(7), 261—266)
[7]	Jia B., Zhang X.L., Ding J. H., Yang S. P., Chen H. W., Chin. Sci. Bull., 2012, 57, 1918—1927
	(贾滨, 张兴磊, 丁健桦, 杨水平, 陈焕文. 科学通报, 2012, 57, 1918—1927)
[8]	Pang S. S., Zhao N., Ouyang Y. Z., Huang K. K., Ding J. H., Chen H. W., Yuan L., Wang X. X., Chem. J. Chinese Universities,2013, 34(6), 1379—1384
	(潘素素, 赵娜, 欧阳永中, 黄科科, 丁健桦, 陈焕文, 袁龙, 王兴祥. 高等学校化学学报, 2013, 34(6), 1379—1384)
[9]	Zhou Z. Q., Jin M., Ding J. H., Zhou Y. M., Zheng J., Chen H. W., Metabolomics,2007, 3(2), 101—104
[10]	Xu N., Zhu Z. Q., Yang S. P., Wang J., Gu H. W., Zhou Z., Chen H. W., Chin. J. Anal. Chem., 2013, 4, 523—528
	(许柠, 朱志强, 杨水平, 王姜, 顾海巍, 周振, 陈焕文. 分析化学, 2013, 4, 523—528)
[11]	Chen H., Zenobi R., Nature Protocols,2008, 3(9), 1467—1475
[12]	Zhu L., Hu Z., Gamez G., Law W. S., Chen H. W., Yang S. P., Chingin K., Balabin R., Wang R., Zhang T. T., Zenobi R., Anal. Bioanal. Chem., 2010, 398(1), 405—413
[13]	Kunitomo J., Journal of Pharmacy(Japanese), 1964, 84(11),1141—1142
	(国友顺一. 药学杂志(日), 1964, 84(11), 1141—1142)
[14]	Kunitomo J., Yoshikawa Y., Tanaka S., Imori Y., Isoi K., Phytochem., 1973, 12(3), 699—701
[15]	Pan Y., Yang G. M., Cai B. C., Ding G., Chinese Traditional and Herbal Drugs,2004, 35(5), 501—503
	(潘扬, 杨光明, 蔡宝昌, 丁岗. 中草药, 2004, 35(5), 501—503