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Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography Mass Spectrometry

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Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography Mass Spectrometry East Tennessee State University Digital Commons @ East Tennessee State University Electronic Theses and Dissertations Student Works 12-2011 Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography Mass Spectrometry. Archana Racharla East Tennessee State University Follow this and additional works at: https://dc.etsu.edu/etd Part of the Analytical Chemistry Commons Recommended Citation Racharla, Archana, "Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography Mass Spectrometry." (2011). Electronic Theses and Dissertations. Paper 1376. https://dc.etsu.edu/etd/1376 This Thesis - Open Access is brought to you for free and open access by the Student Works at Digital Commons @ East Tennessee State University. It has been accepted for inclusion in Electronic Theses and Dissertations by an authorized administrator of Digital Commons @ East Tennessee State University. For more information, please contact [email protected]. Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography – Mass Spectrometry ___________________________ A thesis presented to the faculty of the Department of the Chemistry East Tennessee State University In partial fulfillment of the requirements for the degree Master of Science in Chemistry __________________________ by Archana Racharla December 2011 _________________________ Dr. Chu-Ngi Ho, Chair Dr. Peng Sun Dr. Ningfeng Zhao Keywords: Onion, High Performance Liquid Chromatography, Gas Chromatography Mass Spectrometry, Flavonoid, Alliin. ABSTRACT Survey of Flavonoids and Their Distribution in Different Kinds of Onions Using High Performance Liquid Chromatography and Gas Chromatography – Mass Spectrometry by Archana Racharla This research is done to determine the distribution of flavonoids in diverse varieties of onions (commercial and wild onions). Reflux extraction method was done on dried onions and the abstracts were analyzed subsequently by high performance liquid chromatography (HPLC) and gas chromatography – mass spectrometry (GCMS). Statistical calculations were done to see if there are significant differences in the varieties of onions studied from the chromatographic profiles obtained. The chromatograms obtained were patterned using visual observations, scatter plot study, correlation co-efficient, and ANOVA to evaluate the significant difference of the distribution of flavonoids in varieties of onions. The organic white onions seem to have closer flavonoids profile to that of natural wild onions with a co- relation coefficient of 0.99 from HPLC data and 0.88 from the GCMS data. The ANOVA results also support these conclusions. However, natural wild onions tend to have more constituents that can be beneficial. 2 DEDICATION I would like to dedicate this work to everyone who encouraged me and gave me the strength to achieve my goals. I dedicate this thesis to Racharla (mom, dad, and brother) and Samala (husband and in-laws) families. I dedicate this thesis to all professors in Department of Chemistry at ETSU for their support and guidance to do better. 3 ACKNOWLEDGMENTS I would like to express my deepest and sincere gratitude to my supervisor Dr.Chu-Ngi Ho for his support, patience, guidance, and kindness throughout my studies. I am very thankful for having him as my advisor. I wish to express my sincere thanks to Dr. Peng Sun and Dr. Ningfeng Zhao for being on my thesis committee and their detailed and constructive comments have made this work a success. I esteemly thank Dr. Ray Mohseni and Mr. Mark Klein who supported me in learning the instrumental techniques throughout my study. My special regards to the faculty for their skills and knowledge that I have acquired throughout my course work, and the staff (Tom Webster and Walt Witt) of chemistry department at ETSU for their support in my graduate education. I would like to acknowledge department of chemistry and department of public health for awarding graduate assistantship. I indebtly thank my loving husband Dr. Mallikarjun Samala for his moral support, understanding and encouragement in every step of my education. I am grateful to my parents Mr. Shankaraiah and Ms. Madhulatha and my father-in-law Mr. Ashalu and my mother-in- law Ms. Amrutha and my sweet brother Avinash for their support and prayers. Finally, I would like to thank my friends, my fellow graduate students, and undergraduate students for their support. 4 CONTENTS Page ABSTRACT…………………………………………………………………………………...2 DEDICATION………………………………………………………………………………...3 ACKNOWLEDGEMENTS…………………………………………………………………...4 LIST OF TABLES…………………………………………………………………………….8 LIST OF FIGURES……………………………………………………………………………9 Chapter 1. INTRODUCTION…………………………………………………………………...10 Botany of Onion………………………………………………………………….10 Taxonomy of Onion…………………………...………………………………....11 The Chemical Composition and Chemistry of Allium Cepa.L……………….…12 Medicinal Properties and Uses of Onion…………………………..…………….16 2. METHODS OF FLAVONOID ANALYSIS………………………………………...18 Sample Preparation Techniques for Flavonoid Analysis………………………...18 Pressurized Liquid Extraction………………………………………………..18 Matrix Solid-Phase Dispersion……………………………………………….19 Supercritical Fluid Extraction………………………………………………..19 Microwave-Assisted Extraction……………………………………………...20 Solid Phase Extraction…………………………………………………….....20 Solid Phase Micro-Extraction………………………………………………..21 Ultrasonic Liquid Processor………………………………………………….21 5 Techniques for Separation and Identification of Flavonoids…………………….22 Chromatographic Techniques………………………………………………...22 Thin Layer Chromatography………………………………………....22 Gas Chromatography………………………………………………....23 High Performance Liquid Chromatography……………………….…25 Electrophoretic Techniques…………………………………………………..26 Capillary Electrophoresis…………………………………………….26 3. EXPERIMENTAL METHODS AND PROCEDURES…………………………..…28 High Performance Liquid Chromatography Process…………………………..…28 Isocratic Flow versus Gradient Elution…………………………………..…..29 Normal Verses Reversed Phase HPLC……………..………………………..30 HPLC Columns……….……………………………………………………...31 Detector Used in HPLC…………………………………………………..…..31 Use of Surfactants in HPLC…...………………………………………….….34 Gas Chromatography Process……………………………………………………36 Detector Used in GC…………………………………………...…………….36 Columns Used in GC………………………………………………………....39 Resolution of Bands……………………………………………………………...40 Method Development…………………………………………………………….41 Research………………………………………………………………………….42 4. EXPERIMENTAL PROCEDURES……………………………………………..…..43 Reagents…………………………………………………………………….…....43 Onion Samples...………………………………………………………………....43 Procedures………………………………………………………………..……....44 Preparation of Solutions……………………………………………………...44 6 Preparation of Onion Stock Samples…………………………………………44 Preparation of Standard Stock Samples……………………………………...46 HPLC Instrumentation……………………………………………………………….46 GCMS Instrumentation……………………………………………………………....48 Data Analysis………………………………………………………………………...49 5. RESULTS AND DISCUSSION…………….……………………………………….51 Optimization of Mobile Phase with Surfactants in HPLC…..…………..………...…51 Chromatograms of Onion Samples……………………...…………...………………52 Scatter Plot Study …………………………………………………………................59 Statistical Analysis…………………………………………………………………...64 6. CONCLUSIONS……………………………………………………………………..70 REFERENCES…………………………………………………………………….....73 VITA………………………………………………………………………………....78 7 LIST OF TABLES Table Page 1. Scientific classification of garden onion………………………………………….…12 2. HPLC parameters used for separation and analysis of flavonoids……………….….47 3. GCMS parameters used for separation and analysis of flavonoids………….……....48 4. Averaged retention times and their relative standard deviations from the HPLC chromatograms of the onion samples ……………..………………………………...62 5. Averaged retention times and their relative standard deviations from the GC-MS chromatograms of the onion samples …………….………………..………………...63 6. Correlation coefficients of the samples obtained from the HPLC chromatograms….65 7. Correlation coefficients of the samples obtained from the GCMS chromatograms…65 8. ANOVA p-values of the samples obtained from the HPLC chromatograms…..……68 9. ANOVA p-values of the samples obtained from the GC-MS chromatograms………68 8 LIST OF FIGURES Figure Page 1. Chemical structures of some sulfoxides from the Allium plants…………………....13 2. Enzymatic hydrolysis of Alliin to Allicin. Allicin further decomposes into sulfur compounds…………………………………………………………………………...14 3. Examples of flavonoids from Allium plants………………………………………....15 4. Examples of surfactants that are commonly used in determination of compounds….35 5. Schematic representation of High Performance Liquid Chromatography…………...47 6. Schematic representation of gas chromatographic instrumentation……………..…..49 7. HPLC chromatograms of myricetin, isorhamnetin, quercetin dydrate and quercetin 3- β-D glucoside………………………………………………………………………...52 8. HPLC chromatogram of commercial yellow onion sample……………...…………..53 9. HPLC chromatogram of commercial organic white onion sample……..………...…54 10. HPLC chromatogram of commercial organic red onion sample……………………..54 11. HPLC chromatogram of natural wild onion sample………...……………………….55 12. GCMS chromatogram of commercial yellow onion sample…………………………57 13. GCMS chromatogram of commercial white onion sample…………………………..57 14. GCMS chromatogram of commercial red onion sample……………………………..58 15. GCMS chromatogram of natural wild onion
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