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A General Study of the Effects of Lipids Upon the Quantity of Peroxides Produced by Photosensitized Zinc Oxide

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A General Study of the Effects of Lipids Upon the Quantity of Peroxides Produced by Photosensitized Zinc Oxide A GENERAL STUDY OF THE EFFECTS OF LIPIDS UPON THE QUANTITY OF PEROXIDES PRODUCED BY PHOTOSENSITIZED ZINC OXIDE DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By FREDERICK CLAIRE BLUBAUGH, B.S., B.S. in Phar., M.S. The Ohio State University 1955 Approved by: Adviser College of Pharmacy ACKNOWLEDGMENT The appreciation and gratitude of this author is expressed to Dr. Earl P. Guth, Professor, College of Pharmacy, under whose guidance this research has been per- foiroed, for his invaluable aid given to me. To Dr. B. V. Christensen, Dean, College of Pharmacy, for his advice and guidance and for the opportunity to continue by rendering to me the necessary financial assistance. To Drs. Loyd E. Harris, Frank W. Bope, and John W. Nelson of the College of Pharmacy for their invaluable assistance. To Dr. C. A. Randles, Department of Bacteriology, for his services. My deepest appreciation and gratitude to my wife, Mary Catherine, and to the children, Carol, Barbara, Susan, and M a r g a r e t . ii TABLE OF CONTENTS PAGE INTRODUCTION ..................................... 1 CALAMINE ........................................ 4 ZINC O X I D E ....................................... 5 ZINC OXIDE AS A PHOTOSENSITIZER.................... 7 ULTRAVIOLET LIGHT................................... 10 PROPERTIES OF THE O I L S .............................. 11 OLIVE O I L ..................................... 14 EXPRESSED ALMOND OIL............................ 16 PEACH KERNEL OIL................................ 17 CASTOR OIL..................................... 18 LARD OIL. .............................. 18 COTTONSEED OIL..................................19 SESAME OIL..................................... 20 LINSEED O I L ................................... 21 COD LIVER O I L ..................................22 LIQUID PETROLATUM ............................ 24 SQUALENE........................... 25 PEROXIDES........................................... 25 MATERIALS........................................... 27 ASSAY OF THE OILS................................... 29 EXPERIMENTAL: PREPARATION OF SAMPLES.......................... 30 METHOD OF IRRADIATION ........................ 31 iii TABLE OP CONTENTS (CONT'D) PAGE METHOD OP ASSAY .................. 32 IRRADIATIONS ............................ 33 DISCUSSION................................. 51 SUMMARY.................................... 82 REFERENCES................................. 84 AUTOBIOGRAPHY ............................. 88 iv A GENERAL STUDY OP THE EFFECTS OF LIPIDS UPON THE QUANTITY OF PEROXIDES PRODUCED BY PHOTOSENSITIZED ZINC OXIDE INTRODUCTION Zinc Oxide is a common ingredient of many medicinal products used in the treatment of a wide variety of derma- tological conditions. It is official in the Pharmacopeia of the United States, XIV (41), as Zinc Oxide and in prepar­ ations such as Calamine, Calamine Lotion,! Zinc Oxide Ointment, and Zinc Oxide Paste. In the National Formulary, IX (3 6), it is found in the form of Prepared Neocalamine, Neocalamine Lotion, Neocalamine Liniment, Neocalamine Ointment, Phenolated Neocalamine Lotion, Calamine Liniment, Calamine Ointment, Phenolated Calamine Lotion, Zinc Oxide Hard Paste, Zinc Oxide Soft Paste, and Zinc Oxide Paste with Salicylic Acid. In commerce Zinc Oxide is used in many products similar in composition to the official products as well as many modifications. In addition physicians prescribe this compound freely in many combinations containing fats, hydrocarbons, water, glycols, phenols, and many other types of materials. Reese (51), Mathias (32), and Minardi (34) have studied the "Formation of Hydrogen Peroxide in Calamine Lotions," "The Effect of Various Phenols on the Formation of Hydrogen Peroxide by Zinc Oxide," and "The Effect of Time on the Hydrogen Peroxide Production by Calamine Lotions," respec­ tively. Their studies were devoted exclusively to suspen­ sion of zinc oxide in water preparations. This study is with emulsion type of preparations containing zinc oxide. All of the emulsions were water in oil type except Mineral Oil wherein the zinc oxide apparently functions as an emul­ sifier due to its particle size. The irradiation procedures employed by Reese, Mathias, and Minardi were modified to make them adapted to the study of the water in oil type of emulsion. Reese (51) showed that peroxides were produced in Cala­ mine Lotions upon irradiation with ultraviolet light. Vari­ ous ingredients such as phenol, glycerin, polyethylene glycols, Spans and propylene glycol alginates were shown to have a pronounced effect upon the quantity of peroxide pro­ duced. The addition of ferric oxide to the lotions was detrimental to peroxide production. Reese also found that the light source for peroxide production could be either an ultraviolet lamp, incandescent lamp, fluorescent lamp, or sunlight. Mathias (32) found wide variations in the quantity of peroxides produced in commercial brands of Calamine Lotions when subjected to ultraviolet irradiation. He studied the effect of adding phenol, resorcinol, resorcinol monoacetate and pyrogallol to the suspension. Although his results indicated that the amount of peroxides could be significantly altered, the evidence indicated that there is an optimum concentration of peroxide beyond which any increase in the amount of "additive" results in a decrease in the quantity of peroxide that could be produced. The effect of the addition of various pharmaceutical adjuvants has been shown by Minardi (3*0 to effect markedly peroxide production. Minardi concluded that the addition of either dioctyl sodium sulfosuccinate and/or sodium car- boxymethylcellulose depressed peroxide production. All previous research has been devoted to "lotion" type preparations containing zinc oxide and calamine. Since zinc oxide and calamine are also incorporated into many oifatments and liniments with either a fixed oil or petrola­ tum, a comparative study of the effect of these materials upon the quantity of peroxides produced by photosensitized zinc oxide was in order. Most of the fixed oils used in dermatological practice were selected for this study. CALAMINE During the nineteenth century, the teiro "calamine" was applied by mineralogists Indiscriminately to two minerals, scarely distinguishable by their external characteristics, the carbonate and the silicate of zinc (11). The mineralo­ gist applies the term "calamine" to a hydrous zinc silicate while the carbonate of zinc is known as "Smithsonite." (10) When native zinc carbonate is calcined, an impure zinc oxide remains. This product was teiroed "prepared calamine" in the supplement to the British Pharmacopaeia of 1867 (10). The National Formulary IV, 1916 (38), defined Prepared Cala­ mine as “Native zinc carbonate containing a varying amount of zinc silicate calcined at a moderate temperature; or calcined zinc carbonate, containing a small amount of fer­ ric oxide." The United States Pharmacopeia, XIV (41), defines Calamine as "Zinc oxide with a small amount of ferric oxide." The Merck Index, 6th Edition (33)* lists Calamine (Prepared Calamine) as zinc oxide with about 0.5$ ferric oxide. Calamine is used in medicine only as an external appli­ cant, being employed as a mild astringent and exsiccant in excoriations and superficial ulcerations (11). Apart from its color, which may have some aesthetic value, Calamine U.S.P.has no special advantage over Zinc Oxide U.S.P. (49). Goodman (19) suggested that zinc oxide be substituted for calamine in lotions and other preparations. While Calamine U.S.P. "is zinc oxide with a small amount of ferric oxide," the British Calamine "is a basic zinc carbonate suitable colored with ferric oxide" (4). Calamine Liniment, N.F. IX, served as the initial phar­ maceutical preparation for this study. It first appeared in the N.F. V, 1926 (37)* and has remained unchanged in all revisions of the N.F. ZINC OXIDE The Pharmacopeia of the United States, XIV (41), states that "Zinc oxide, freshly ignited, contains not less than 99 per cent ZnO." The method of its manufacture or its crystalline structure are not specified. Freedom from im­ purities especially of lead and arsenic are of prime impor­ tance. The commercial production of zinc oxide was started by LeClair and Sorel in France during the latter part of the eighteenth century, employing the prodess now known as the French Process or the two step process. In the United States, commercial production was started by Weatherill and Jones about 1 8 5 5. The American process was based on an observa­ tion made by a workman who noticed white fumes given off from zinc ores while repairing a break in a boiler flue. This process is now known as the American Process or the direct process (39). The French Process involves burning of slab zinc metal (spelter) with air. The zinc metal is heated in a retort to the boiling point. When the zinc vapors come in contact with air, they b u m with a bright yellowish colored flame to produce zinc oxide. These fumes are carried through suit­ able conduits to settling chambers. The physical properties of the oxide may be controlled within certain limits by the rate of oxidation, but the particle shape is characteristic­ ally spherical. The basic principle of the American Process is to vaporize the zinc directly from zinc ores rather than from the metal since the oxide possesses the property of passing from the solid state directly to the vapor state and back again to
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