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Trisiloxane Surfactant Adjuvants in Pollen

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Trisiloxane Surfactant Adjuvants in Pollen Utah State University DigitalCommons@USU All Graduate Theses and Dissertations Graduate Studies 8-2020 Trisiloxane Surfactant Adjuvants in Pollen Autumn Slade Utah State University Follow this and additional works at: https://digitalcommons.usu.edu/etd Part of the Environmental Engineering Commons Recommended Citation Slade, Autumn, "Trisiloxane Surfactant Adjuvants in Pollen" (2020). All Graduate Theses and Dissertations. 7909. https://digitalcommons.usu.edu/etd/7909 This Thesis is brought to you for free and open access by the Graduate Studies at DigitalCommons@USU. It has been accepted for inclusion in All Graduate Theses and Dissertations by an authorized administrator of DigitalCommons@USU. For more information, please contact [email protected]. TRISILOXANE SURFACTANT ADJUVANTS IN POLLEN by Autumn Slade A thesis submitted in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE in Environmental Engineering Approved: ______________________ ____________________ William J. Doucette, Ph.D. Diana Cox-Foster, Ph.D. Major Professor Committee Member ______________________ ____________________ Laurie McNeill, Ph.D. Janis L. Boettinger, Ph.D. Committee Member Acting Vice Provost for Graduate Studies UTAH STATE UNIVERSITY Logan, Utah 2020 ii Copyright © Autumn Slade 2020 All Rights Reserved iii ABSTRACT Trisiloxane Surfactant Adjuvants in Pollen by Autumn Slade, Master of Science Utah State University, 2020 Major Professor: Dr. William J. Doucette Department: Civil and Environmental Engineering Trisiloxanes surfactants (TSSs), used as adjuvants in agricultural applications worldwide, are presumed to be biologically inert. However, recent studies indicate that TSSs may have direct negative impacts on bees, in addition to synergistic negative effects when associated with pesticides and viruses. TSSs have been found in surface waters, pollen, and beeswax, but their environmental prevalence and fate are not well understood, in part, because of the analytical difficulty associated with the quantification of the complex commercial adjuvant mixtures. To assess the prevalence and concentrations of TSSs in pollen collected by bees, samples collected from pollen traps were analyzed for three different TSSs oligomer groups (TSS-H, TSS-COCH3, and TSS-CH3) using liquid chromatography tandem mass spectrometry (LCMS/MS), as well as 60+ pesticides. Of the 99 pollen samples analyzed, TSS-H and a TSS-COCH3 like substance were found in 43% and 15% of pollen respectively, along with nine pesticides. No TSS-CH3 was found. Experiments were performed to examine the volatilization and hydrolysis of iv TSSs, in addition to long term recoveries of TSSs from spiked or fortified pollen. Plant uptake studies were also performed to assess the transfer of TSSs from roots to flowers. Headspace GCMS experiments did not observe significant volatilization of TSSs but did tentatively identify several low molecular, linear volatile silicone compounds. Hydrolysis half-lives of TSSs were less than 2 days in acidic and basic aqueous solutions and less than 5.9 days at a neutral pH. The long-term recovery of TSSs in pollen was low and with sorption to pollen and polypropylene occurring. The potential transfer of TSSs from roots to flowers was relatively low based on the results of the pressure chamber studies, but TSSs were identified in the flowers of plants exposed to repeated high exposures in whole plant hydroponic studies. TSSs also did not significantly impact the root to shoot transfer of cyprodinil, one of the pesticides found in the pollen survey samples. (120 pages) v PUBLIC ABSTRACT Trisiloxane Surfactant Adjuvants in Pollen Autumn Slade Chemicals are often added to agricultural pesticide mixes to help increase the efficiency of the field spray solution, and one of the main groups of chemicals used for this purpose are trisiloxane surfactants (TSSs). Normally TSSs are considered non-toxic, but recent studies have shown TSSs to have negative impacts on organisms like honey bees. Though TSSs have recently been found in environmental sources like water, pollen, and beeswax, little is known about how TSSs behave in the environment or affects active ingredients, like pesticides. To help determine the environmental prevalence and fate of TSSs, several studies were performed. Pollen was collected from across the United States and analyzed for TSS-H, TSS-COCH3, and TSS-CH3, where TSS-H and a TSS-COCH3 like compound were found, along with nine pesticides. The likelihood for TSSs to be found in the air, water, roots, and plants was looked at as well. TSSs were determined to not be of a great concern in the air and were rapidly degradable in water in basic or acidic conditions with half of the compound disappearing in less than two days. TSSs were also found to sorb to many different surfaces, including pollen and polypropylene, a type of commonly used plastic. Lastly, TSSs were not found to readily travel from plant root solution to the leaves and flowers. This means that overall, TSSs are not stable in the environment and are not likely to travel into pollen at significant concentrations except potentially through direct contact onto the pollen or repeat exposures to the roots or leaves. vi ACKNOWLEDGMENTS First and foremost, I would like to thank Dr. William Doucette, my advisor, for his patience with all of the times I’ve interrupted him in his office with questions. Without his good advice, encouragement, and guidance, this thesis would never have been finished. I would also like to thank my committee members, Dr. Diana Cox-Foster and Dr. Laurie McNeill for their time they gave and the knowledge they’ve shared. I am grateful for the American Honey Producers Association who started and funded a large portion of this project, as well as the Utah Water Research Laboratory, the USDA-ARS Pollinating Insect-Biology Research Unit, and the Crop Physiology Laboratory who helped provide research facilities and materials, as well as knowledge in their various areas of expertise. I’d specifically like to thank Ellen Klinger and Mary-Kate Williams for their help with pollen samples and analysis, Joe Stewart for his guidance and technical assistance, and Terri Manwaring, Alec Hay, and Bruce Bugbee for their assistance in plant growth. Thanks to all the friends and family who’ve supported me through my academic career and had the patience to listen to me rant about things I’m interested in, even if they aren’t interested or don’t entirely understand what I’m talking about. Lastly, a shout out of gratitude to my parents for their support, love and encouragement they give me to make my own path and follow my interests. Autumn Slade vii CONTENTS Page ABSTRACT ...................................................................................................................... iii PUBLIC ABSTRACT .........................................................................................................v ACKNOWLEDGMENTS ................................................................................................ vi LIST OF TABLES ............................................................................................................ ix LIST OF FIGURES .......................................................................................................... xi CHAPTER I. INTRODUCTION ..................................................................................................1 Objectives ................................................................................................................3 II. LITERATURE REVIEW ......................................................................................4 Use of Trisiloxane Surfactant Adjuvants .................................................................4 Characterization of Trisiloxane Surfactants.............................................................5 Toxicities of Trisiloxane Surfactants .......................................................................7 Environmental Concentrations of Trisiloxane Surfactants ......................................9 Environmental Fate of Trisiloxane Surfactants .....................................................11 Plant Uptake and Surfactant Effects on Pesticidal Uptake ....................................13 III. DEVELOPMENT OF ANALYTICAL METHODS FOR TSS EXTRACTION AND ANALYSIS ...........................................................................................17 Methods and Materials ...........................................................................................17 Results ....................................................................................................................22 Analysis of Impurities, Hydrolysis Products, and Pesticides ................................26 IV. 2018 POLLEN STUDY .....................................................................................28 Methods and Materials ...........................................................................................28 Results ....................................................................................................................30 V. ADDITIONAL LONG-TERM RECOVERIES ..................................................35 Methods and Materials ...........................................................................................35 Results ....................................................................................................................36 VI. POTENTIAL LOSSES OF TSS FROM LONG-TERM POLLEN SPIKES .....42 Materials
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