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Isolation and Characterization of Floc-Causing Substances in Granulated Cane Sugar

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Isolation and Characterization of Floc-Causing Substances in Granulated Cane Sugar Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1975 Isolation and Characterization of Floc-Causing Substances in Granulated Cane Sugar. Huan-wen Herbert Hsu Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Hsu, Huan-wen Herbert, "Isolation and Characterization of Floc-Causing Substances in Granulated Cane Sugar." (1975). LSU Historical Dissertations and Theses. 2834. https://digitalcommons.lsu.edu/gradschool_disstheses/2834 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. INFORMATION TO USERS This material was produced from a microfilm copy of the original document. While the most advanced technological means to photograph and reproduce this document have been used, the quality is heavily dependent upon the quality of the original submitted. The following explanation of techniques is provided to help you understand markings or patterns which may appear on this reproduction. 1. The sign or "target" for pages apparently lacking from the document photographed is "Missing Page(s)". If it was possible to obtain the missing page(s) or section, they are spliced into the film along with adjacent pages. This may have necessitated cutting thru an image and duplicating adjacent pages to insure you complete continuity. 2 . When an image on the film is obliterated with a large round black mark, it is an indication that the photographer suspected that the copy may have moved during exposure and thus cause a blurred image. 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Xerox University Microfilms 300 North Zeeb Road Ann Arbor, Michigan 48106 76-148 HSU, Huan-Wen Herbert, 1937- ISOLATION AND CHARACTERIZATION OF FLOC-CAUSING SUBSTANCES IN GRANULATED CANE SUGAR. The Louisiana State University and Agricultural and Mechanical College, Ph.D., 1975 Food Technology Xerox University Microfilms,Ann Arbor, Michigan 48106 THIS DISSERTATION HAS BEEN MICROFILMED EXACTLY AS RECEIVED. ISOLATION AND CHARACTERIZATION OF FLOC-CAUSING SUBSTANCES IN GRANULATED CANE SUGAR A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Food Science by Huan-Wen Hsu B.S., Taiwan Provincial Maritime College, 1967 M.S., Louisiana State University, 1972 August, 1975 ACKNOWLEDGMENTS The author wishes to express his sincere gratitude for the guidance and assistance rendered to him in this en­ deavor by his major professor, Dr. Joseph A. Liuzzo of the Department of Food Science, Louisiana State University. He also acknowledges his appreciation to Dr. Arthur F. Novak, Head of the Department of Food Science, for his encourage­ ment during the course of this investigation. He wishes to thank the following organizations for their cooperation in supplying sugar samples: Coca-Cola Company; Refined Syrups and Sugars, Inc.; Southdown Lands Inc.; Supreme Sugar Refining; Revere Sugar Refinery; Savannah Sugar Refining Corporation; and Imperial Sugar Company. ii TABLE OF CONTENTS ACKNOWLEDGMENTS ..................................... ii LIST OF T A B L E S ............ iv LIST OF FIGURES..................................... v ABSTRACT ........................................ viii INTRODUCTION ...... 1 LITERATURE REVIEW ................................... 3 MATERIALS AND METHODS ............................... 11 RESULTS AND DISCUSSION ............................ 32 SUMMARY............................................. 94 BIBLIOGRAPHY.......................... 96 VITA ............................................... 99 iii LIST OF TABLES Table Page 1. The Results of the Acid Floe, the Alcohol Floe, and the Soft Drink Beverage Tests . 34 2. Acid Floe Formation Time Related to Temperature .............................. 37 3. Acid Floe Formation Time in Relation to the Kind of Acid A d d e d .................... 37 4. Floe Formation Time in Relation to Solution p H .............................. 39 5. Effect of Heating on Time of Acid Floe F o r m a t i o n ............................ 40 6. Effect of EDTA on Floe Formation ....... 42 7. Extraction of the Alcohol Precipitates of Floc-Positive Sugars ...................... 44 8. Absorption Bands and Related Vibration Groups Useful in Floe Investigation.............. 86 9. Floe Formation Time Related to the Volume of Formaldehyde Added to Sugar Solutions . 90 10. Comparison of the Floe Formation Time between Methylated FCS and Non-Methylated FCS . 92 iv LIST OF FIGURES Figure Page 1. A comparison of extraction methods for the floc-causing substance .............. 19 2. Scheme Number 1 for the isolation of the floc-causing substance .................. 21 3. Scheme Number 2 for the isolation of the floc-causing substance .................. 22 4. The type of acid floe from a floc-positive s u g a r ..................................... 35 5. The Dowex 50W-x2 fractionation of an alkaline extract of a one-week-old Aust.R. sugar alcohol precipitate ...................... 46 6. Dowex 50W-x2 fractionation of FCS from a two-month-old alcohol precipitate of Aust.R. sugar ...................... 47 7. Iodine tests of the Dowex 50W-x2 fractions which were fractionated from a one-week-old alcohol precipitate of the Aust.R. sugar . 49 8. Folin Phenol reagent test of the Dowex 50W-x2 fractions which were fractionated from a one-week-old precipitate of the Aust.R. s u g a r .................................... 50 9. Phenol-sulfuric acid tests of the Dowex 50W-x2 fractions which were fractionated from a one-week-old precipitate of the Aust.R. s u g a r .............. 51 10. The Dowex 50W-x2 fractionation results of a two-month old alcoholic precipitate of sugar (sample Jap) solution............. 53 11. Results of the iodine test on the Dowex 50W-x2 fractions of a two-month-old alcoholic precipitate of a Japanese sugarsolution . 54 v 12. Results of the Folin phenol reagent test on the Dowex 50W-x2 fractions of a two-month-old alcoholic precipitate of a Japanese sugar solution................................... 55 13. Results of the phenol-sulfuric acid test for general carbohydrates in the Dowex 50W-x2 fractions of a two-month-old precipitate of a Japanese sugar solution . .............. 56 14. Results of the elution of the Dowex 50W-x2 column fraction 3 from Amberlite IR-45 (0H~) 59 15. Floccing results of the fractions from the alkalized extract of the methanol extracted alcohol precipitate ...................... 61 16. Iodine test results of fractions from the alkalized extract of the alcoholic precipi­ tate of the Aust.R. sugar which was pre­ viously extracted with methanol .......... 63 17. Folin phenol test results of the fractions from the alkalized extract of the alcoholic precipitate of the Aust.R. sugar which was previously extracted with methanol ........ 64 18. Phenol-sulfuric acid test results of fractions from the alkalized extract of the alcoholic precipitate of the Aust.R. sugar which was previously extracted with methanol ........ 65 19. The results of floe formation of the fractions from the Sephadex G-150 c o l u m n ............ 67 20. The iodine test results of fractions from the Sephadex G-150 column .................... 68 21. The phenol-sulfuric acid test results of the fractions from the Sephadex G-150 column . 69 22. Carbohydrate paper chromatographic results of hydrolyzed undialyzable FCS from fraction IF.18 ............................ 71 23. Carbohydrate paper chromatographic results of hydrolyzed FCS from fraction 2F.3 and IF.18 72 24. Paper chromatographic results of amino acids in Aust.R. and Jap hydrolysates of fraction IF. 18 .................. 73 vi 25. Paper chromatographic results of sugars in enzyme hydrolyzed fractions from the Amberlite IR-45 ..... 74 26. Paper chromatographic results of sugars in enzyme hydrolyzed fractions of Aust.R. from the Amberlite IR-45 column ................ 75 27. Cellulose TLC for uronic acid determination of hydrolyzed Jap and Aust.R. fractions . 76 28. An amino acid chromatogram of the FCS's in Aust.R. and Jap fractions 2F . 3 ............. 77 29. The effect of acid concentration and time of hydrolysis on the yield of amino acids from Amberlite IR-45 fractionation of Aust.R. 79 30. Amino acid content
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