Asparagus Officinalis L. 24 h. ambient ionization mass spectrometry CHINESE JOURNAL OF APPLIED CHEMISTRY Apr Asparagus Officinalis L

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1 33 4 Vol. 33 Iss CHINESE JOURNAL OF APPLIED CHEMISTRY Apr a a b a* a b Asparagus Officinalis L ieesi-ms CH 3 OH m /z 50 ~ 1000 CID 1 min O652 A DOI /j. issn Asparagus Officinalis L h 3 β P 8 ambient ionization mass spectrometry 9 MPT IRT BCB24005 KJLD13051 Tel /Fax chw8868@ gmail. com

2 LTP 11 DART 12 SDAPCI 13 LAESI 14 DESI 15 AFAI 16 EESI 17 paper spray 18 ieesi-ms ieesi- MS ieesi- MS ieesi LTQ-XL Xcalibur Thermo Scientific mm mm Agilent Technologies ROE m /z 50 ~ kv V 65 V 1. 5 Da 10% ~ 30% 30 ~ 50 ms LTQ-Tune 1. 2 A B C D 4 ieesi-ms 1 min 1. 3 ieesi-ms ieesi-ms CH 3 OH 3 ~ 5 μl /min 2 mm 5 mm 1 1 Fig. 1 ieesi-ms Schematic diagram of ieesi-ms

3 ieesi-ms ieesi-ms 2 2A 2B 2C2D A B C D ieesi-ms K + Na + M + K + M + Na + 20 / CID ieesi-ms / glucose /fructose MW180 sucrose MW342 m /z 219 glucose / fructose + K + m /z 381 sucrose + K + m /z 399 sucrose + K + H 2 O + m /z 561 glucose / fructose + sucrose + K + m /z 707 2sucrose + Na + 21 m /z 175 arginine + H + m /z 104 choline + MW170m /z 171 undecanal + H + MW184m /z 185 lauraldehyde + H +3 2 A A B B C CD D ieesi-ms Fig. 2 ieesi-ms spectra of fresh asparagus tubers subcutaneous tissue of AA BB CCand DDsegments which were cut out subsequently from the bottom to the top of asparegus ieesi-ms / glucose /fructose MW180 sucrose MW342 m /z 219 glucose /fructose + K + m /z 381 sucrose + K + m /z 399 sucrose + K + H 2 O + m /z 561 glucose /fructose + sucrose + K + m /z 104 choline + m /z 171undecanal + H + m /z 185 lauraldehyde + H ieesi-ms 3 ieesi-ms 3A 3B 3C3D A B C D ieesi-ms m /z 219 glucose /fructose + K + m /z 381 sucrose + K + m /z 399 sucrose + K + H 2 O + m /z 175 arginine + H + m /z 104 choline + m /z 171 undecanal + H + m /z 185 lauraldehyde + H + m /z

4 A A B B C CD D ieesi-ms Fig. 3 ieesi-ms spectra of fresh asparagus epidermal tissue of AA BB CCand DDsegments which were cut out subsequently from the bottom to the top of asparegus m /z 976 CID m /z Da m /z 976 m /z 649 rutin MW610M + K + 5 P 2. 3 ieesi-ms ieesi-ms 4 4A 4B 1 2 m /z m /z 219 glucose /fructose + K + m /z 399 sucrose + K + H 2 O + m /z 399 sucrose + K + H 2 O + m /z 381 sucrose + K + H 2 O m /z 700 ~ 900 m /z CID PC34 2+ K + PC36 4+ K m /z 175 arginine + 4 ieesi-ms Fig. 4 ieesi-ms spectra of two types of dry asparagus H + 1 tubers m /z 116 proline + H + A. rhizomeb. stem tip m /z 104 choline +

5 4 485 m /z 104 m /z 171 undecanal + H + m /z 185 lauraldehyde + H CID 5 A B C DMS 2 CID m / z 104 choline + m /z OH CHOHCH 2 5A m /z 171 undecanal + H + m /z OH CH 2 CH 2 O 5B m /z 175 arginine + H + m /z NH 3 17 H 2 O 18 COOH 45 NH CNH C 23 m /z 219 glucose + K + m /z H 2 O18 C 3 H 5 O 3 5D MS 2 CID m /z 104 A m /z 171 B m /z 175 C / m /z 219 DMS /MS Fig. 5 The MS 2 spectra of cholinem /z 104 A undecanalm /z 171 B argininem /z 175 Cand glucose m /z 219 Dfrom asparagus tissue 1 Table 1 ieesi-ms /MS The characteristic product ions of ieesi-ms / MS from asparagus tissue Cmpound Molecular structure Observed m /z Ion formation FragmentsMS /MS Undecanal Continued on next page O 154M + H - OH M + H + CH 3 CH 2 8 CH 2 H 127M + H - CH 2 CH 2 O +

6 continued from previous page Cmpound Molecular structure Observed m /z Ion formation FragmentsMS /MS Proline 116 M + H + 70M + H - H 2 O - CO M - OH + Choline 104 M 60M - CH 2 CH 2 O + Sucrose 342 M + K + 363M + K - H 2 O + 345M + K - 2H 2 O + 219M + K - Glu + 201M + K - Glucose + Serine H 2 O NCHCOH CH2 OH + 88M + H - H 2 O M + H 60M + H - H 2 O - CO + 158M + H - NH 3 + Arginine 175 M + H + 157M + H - H 2 O + 130M + H - COOH + 116M + H - NH = CCNH Glucose 219 M + K + 201M + K - H 2 O + 130M + K - C 3 H 5 O ieesi-ms SDAPCI-MS 13 LAESI-MS 14 Leaf spray- MS 21 ieesi-ms ieesi DESI SDAPCI ieesi-ms ieesi-ms 19 4 ieesi-ms 1 min 1LI Cuixia MAO Ruoqing LI Zhizhong et al. Composition Analysis and Nutritional Evaluation of the Asparagus J. Mod

7 4 487 Food Sci Technol in Chinese.. J SUN Chunyan ZHAO Botao YU Zhifang et al. The Development of Chemical Components in Asparagus Officinalis and Their Medical Effects J. Chinese Wild Plant Resour in Chinese.. J KANG Xu YUAN Jianglan DENG Chuan et al. Analysis of Volatile Flavour Components in Green Asparagus Tea by GC- MS J. Farm Prod Process in Chinese.. GC-MS J Kim B Y Cui Z G Lee S R et al. Effects of Asparagus Officinalis Extracts on Liver Cell Toxicity and Ethanol Metabolism J. J Food Sci H Wang M F Tadmor Y Wu Q L et al. Quantification of Protodioscin and Rutin in Asparagus Shoots by LC / MS and HPLC methods J. J Agric Food Chem Zhong C Jiang C Xia X et al. Antihepatic Fibrosis Effect of Active Components Isolated from Green AsparagusAsparagus Officinalis L. Involves the Inactivation of Hepatic Stellate Cells J. J Agric Food Chem Hafizur R M Kabir N and Chishti S. Asparagus Officinalis Extract Controls Blood Glucose by Improving Insulin Secretion and Beta-Cell Function in Streptozotocin-Induced Type 2 Diabetic Rats J. Br J Nutr Chua L S. A Review on Plant-Based Rutin Extraction Methods and its Pharmacological Activities J. J Ethnopharmacol ZHANG Xie HU Bin CHEN Huanwen. Fundamental Principles and Practical Applications of Ambient Ionization Mass Spectrometry for Direct Analysis of Complex Samples J. Chinese J Anal Chem in Chinese.. J Zhang T Q Zhou W Jin W et al. Direct Desorption / Ionization of Analytes by Microwave Plasma Torch for Ambient Mass Spectrometric Analysis J. J Mass Spectrom Wiley J S Shelley J T Cooks R G. HandheldLow-Temperature Plasma Probe for Portable Point-and-Shoot Ambient Ionization Mass Spectrometry J. Anal Chem Nah T Chan M Leone S R et al. RealTime in Situ Chemical Characterization of Submicrometer Organic Particles Using Direct Analysis in Real Time-Mass Spectrometry J. Anal Chem ZHU ZhiqiangYAN JianpingWANG Yu et al. Surface Desorption Atmospheric Pressure Chemical Ionization Mass Spectrometry for Rapid Analysis of Capmhor Wood ProductsJ. Chinese J Anal Chem in Chinese.. J Shrestha B and Vertes A. High-throughput Cell and Tissue Analysis with Enhanced Molecular Coverage by Laser Ablation Electrospray Ionization Mass Spectrometry Using Ion Mobility Separation J. Anal Chem David Calligaris D C Xiaohui Liu Isaiah Norton et al. Application of Desorption Electrospray Ionization Mass Spectrometry Imaging in Breast Cancer Margin Analysis J. Proc Natl Acad Sci USA Luo Z G He J M Chen Y et al. Air Flow-Assisted Ionization Imaging Mass Spectrometry Method for Easy Whole-body Molecular Imaging under Ambient Conditions J. Anal Chem Chen H W Sun Y P Arno Wortmann et al. Differentiation of Maturity and Quality of Fruit Using Noninvasive Extractive Electrospray Ionization Quadrupole Time-of-flight Mass Spectrometry J. Anal Chem Zhang C Manicke N E. Development of a Paper Spray Mass Spectrometry Cartridge with Integrated Solid Phase Extraction for Bioanalysis J. Anal Chem Zhang H Gu H Yan F et al. Direct Characterization of Bulk Samples by Internal Extractive Electrospray Ionization Mass Spectrometry J. Sci Rep Zhang H Chingin K Zhu L et al. Molecular Characterization of Ongoing Enzymatic Reactions in Raw Garlic Cloves Using Extractive Electrospray Ionization Mass Spectrometry J. Anal Chem Liu J Wang H Cooks R G et al. Leaf SprayDirect Chemical Analysis of Plant Material and Living Plants by Mass Spectrometry J. Anal Chem Guo SWang Y Zhou D et al. Significantly Increased Monounsaturated Lipids Relative to Polyunsaturated Lipids in Six Types of Cancer Microenvironment are Observed by Mass Spectrometry Imaging J. Sci Rep ZHANG Hua ZHU Liang CHEN Huanwen. Direct Molecular Analysis of Garlic Using Internal Extractive Electrospray Ionization Mass Spectrometry J. Chinese J Anal Chem in Chinese.. J Zhang H Zhu L Luo L et al. Direct Assessment of Phytochemicals Inherent in Plant Tissues Using Extractive Electrospray

8 Ionization Mass Spectrometry J. J Agric Food Chem Rapid Analysis of Chemical Composition in Asparagus Using Internal Extractive Electrospray Ionization Mass Spectrometry LU Haiyan a ZHANG Hua a PENG Xiaoming b CHEN Huanwen a* a Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation East China Institute of Techonolgy Nanchang China b Xingguo Xian Boyuan Agricultural Development Co. Ltd. Xingguo Jiangxi China Abstract Rapid analysis chemical composition of plant samples was achieved using internal extractive electrospray ionization mass spectrometryieesi-mswithout any sample pretreatment. In this studyfresh asparagus tubers together with two kinds of dry asparagus tubers were treated as representative samples for the ieesi-ms analysis. Choosing methanol as an ieesi extractantvarious chemical composition in asparagus tissue samples was profiled in mass scan range of m /z 50 ~ 1000 under the positive ion detection modeand through collision-induced dissociation CID experimentsnutrient and medicinal components including sugarsamino acidsalkaloidsand rutin were identifiedwhich play an significant role in development of pharmaceutical drugsnatural product research and understanding of primary and secondary metabolites. Our experimental results demonstrate that ieesi-ms makes rapid recognition of chemical composition differences in different asparagus. Such information renders the nutritious and medicinal assessment of plant natural products possible. The merits of ieesi-ms include no sample pretreatmenthigh-throughput less than 1 min per sample low sample consumptionsimplicityas well as good specificityshowing potential applications in phytochemicals analysis. Keywords asparagusinternal extractive electrospray ionizationmass spectrometrydirect analysis Received Revised Accepted Supported by the National Natural Science Foundation of ChinaNo Program for Changjiang Scholars and Innovative Research Team in UniversityPCSIRT No. IRT13054 Science and Technology Planning Project at the Department of Science and Technology of Jiangxi ProvinceChinaNo BCB24005 Jiangxi Province Program for the support of Science and Technology in UniversitiesNo. KJLD13051 Corresponding authorchen HuanwenprofessiorTel /Fax chw8868@ gmail. comresearch interestsmass spectrometry

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