`
`JOURNAL OF
`FOOD
`ENGINEERING
`
`www.eIsevier.comflocateIjfoodeng
`
`Microwave drying effects on properties of whey protein isolate edible
`films
`
`Sevim Kaya, Ahmet Kaya '
`Food Engineering Department, University of Ga:ian.rep, 27310 Gazitmtep, Turkey
`Received ll December 1998; received in revised form 9 August I999; accepted I3 September I999
`
`Abstract
`
`Whey protein isolate (WPI) edible films were dried using microwave drying or at room conditions. The drying time of the films
`required 5 min in microwave oven and 18 h at room conditions. Water vapor permeability (WVP), mechanical properties, gloss and
`haze of WPI based edible films were determined. Water vapor transmission rate (WVTR) increased with increasing temperature. but
`the results showed that WVP did not show a similar trend. Microwave drying and drying at room conditions gave similar results for
`the WVP. Application of microwave increased the elongation and tensile strength values. (9 2000 Elsevier Science Ltd. All rights
`reserved.
`
`1. Introduction
`
`Edible films and coatings may have potential appli-
`cations in the food industry (Siimnii & Baymdirh, 1995).
`Edible films and coating are generally formed from a
`solution or dispersion of the film-forming agent, fol-
`lowed by any of the several means to separate the film-
`forming agent from the fluid carrier, or by solidification
`of the film-forming material from a melt (Kester &
`Fennema, 1986). Films and coatings may be differenti-
`ated on the basis of an application method. A film can
`be preformed and applied to a food at any time, much
`like a synthetic package, whereas a coating must be
`applied in liquid fonn to a feed directly (Sherwin, I998).
`The specificity of the edible films needs further studies to
`improve the mechanical and barrier properties (Kester
`& Fennema. 1986).
`Whey protein, a by product of cheese manufacture, is
`produced in large quantities and has excellent functional
`properties and could potentially be used for edible films.
`Barrier and mechanical properties of whey protein iso-
`late based films have been studied by some researchers,
`but generally they have been studied at 25°C and 100-
`0% relative humidity (RH) gradient
`(McHugh &
`Krochla,
`l994a; Chen, 1995; Fairley, Monahan, Ger-
`man & Krochta, 1996; Kroehta & De Mulder-Johnston,
`1997). WPI films can be made from 8% to I2"/o whey
`
`° Corresponding author.
`
`protein solutions (Mel-[ugh & Krochta, 1994b). It was
`found that below 8%, WPI intact films were not formed,
`presumably due to lack of intermolecular interactions
`upon film dehydration (McHugh, Aujard & Kroehta,
`I994). On the other hand, after 11% of WPI, whey
`protein solutions become gel during heating. Plastic-
`izers, such as glycerol and sorbitol, are used generally
`for WPI—based edible films to enhance the film flexibility
`and extensibility (Mel-lugh & Krochta, 1994b; McHugh,
`Avena-Bustillos & Krochta,
`I993; Banerjee & Chen,
`1995; Mate. Frankel & Krochta 1996).
`Most types of edible films are prepared by air drying
`(ca. 24 h) after spreading film solution over the plate, a
`fairly rapid film formation is generally required for in-
`dustrial reasons. As microwave drying is one of the
`fastest drying methods, it was thought that microwave
`drying could be applied to dry films.
`One of the most useful functions of edible films is
`
`their ability to act as water, gas (mainly, oxygen and
`carbon dioxide) and oil barriers. Water vapor penne-
`ability is one of the most important and widely studied
`property of edible films. Mechanical properties are as
`important to edible films as barrier properties are. Ad-
`equate mechanical strength ensures the integrity of a
`film and its freedom from minor defects, such as a pin
`hole, which ruin the barrier property (Chen, 1995).
`Tensile strength expresses the maximum stress devel-
`oped in a film during a tensile test and ollers a measure
`of integrity and heavy duty use potential for films and
`percentage elongation at break is a quantitative
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`representation of a film’s ability to stretch (Gennadios,
`Weller & Testin, 1993}.
`The aim of this study is to apply microwave drying
`during preparation of edible films to shorten film drying
`time. The most important factor for applicability of
`dilierent preparation techniques is obtaining similar or
`better properties than usual drying methods. Therefore,
`WVP, tensile strength, elongation,‘ gloss and haze of the
`films were d°_t°"m“ed' S'",°°_the 3"“ °f this Stmiy '5 9°‘
`stlldylng drying, chanfctensncs °_f WPI films flrled with
`microwave or air drying, the drying characteristics were
`nm !nVe5“gm,ed' Further itudfes are “cede?! for '_m'
`proving the microwave application and analyzing drying
`charactensucs‘
`
`2. Materials and methods
`
`2. I. Materials
`
`,
`,
`WPI (BiPro, 98.1% protein) used t0 make films was
`supplied by Davisco lntemational, Le Seur, MN. All
`chemicals used were reagent grade and the water was
`doubly distilled’
`
`2.2. Film formation
`
`Aqueous solutions °f 8% and 10% (Wm) WPI were
`prepared and heated with stirring to 90 :1: 2°C for 15 min
`(total heating time is 30 min) over a hot plate. Solutions
`were cooled to room temperature and vacuum was then
`apphed to remove dissolved ah-_ Glycel-inc (G) was
`added as an equal weight of WPI originally dissolved to
`provide 59% wp1;50% G fihns, mm solids basis_ so_
`lutions containing 2.6 g total solids were pipetted per
`glass plate (15 cmx 15 cm) to minimize thickness vari-
`ations between treatments. Ten plates were cast per
`formula. The solutions were spread evenly with a glass
`rod (Avena-Bustillos & Krochta, 1994} allowed to dry at
`mom conditions (20 3: 20C and 40 i 5% RH) ovemight
`and dried films were peeled from casting surface. Then
`dried films were left at 23 1 2°C and 45 3; 5% RH for
`conditioning for one day.
`the emulsions
`In the case of microwave drying,
`spread over glass plates were dried in a microwave oven
`(Argelik, ARMD 580, with power output 700 W, oper-
`ated at 2450 MHz) for 5 min. The boiling and bubbling
`were not observed during drying. The dried films were
`peeled-ofl‘ and the same conditioning used for the mi-
`crowave dried films was applied.
`
`2.3. Film tliickness
`
`Thickness of films was measured with a micrometer
`
`cut into 3.2 cm diameter circles and thickness of each
`film was measured at six random positions around the
`film following WVP tests. Mean values were used for the
`calculations (SD 1 0.02).
`
`2.4. Water vapor permeability
`
`wmer Vapor transmission of films was measured
`using procedures described by some researchers (Kam-
`per & Fenncma 1984; Aydt, Weller & Testin 1991; Park
`& Chinnan,
`I995; Sherwin, 1998)_ Circular glass test
`cups with a diameter of 3 cm and a depth of 3 cm were
`used_ Am“, placing [0 ml of distilled H20 in each cup’
`they were covered with the edible films. Films were cut
`circularly with a diameter slightly larger than the di-
`ameter of the cup and then they were scaled using
`melted paraflin. The cups were weighed with their con-
`tents and placed in a desiccator containing saturated
`Mg(N0;)2 solution at the bottom. The relative humidity
`I e of saturated M O
`I
`t'
`t
`h t
`iiiluliie range studied \§z(tI: fdiiznflozg l3.r;9a16,ea(‘}:.54;=l8n!:l:1lil
`0514 at 40C’ 20cc and 30aC_ rcspcctively (Labuza,
`1984) The desiccators were kept in the incubator (Niive
`ES 50ll) at 4°C 20°C or 30"C. Cups were weighed up to
`30-40 h. Three replicates of each film were tested.
`Height of air gap between film and desiccant in cups was
`measured initially and finally and relative humidities
`and WVP values were calculated using WVP Correction
`Method.
`
`2.5. The water vapor permeability calculations
`_
`_
`_
`_
`_
`_
`The relative humidity inside the cup was provided as
`100% by Placing the Water into "19 C“P- The 1"-'IatiV°
`h““1Idi"-Y °'“5Id° the “P W‘_‘5 31":-lund 50% by Placing
`53t‘_“‘“°d MB(N03-)2 5°“-'“°“ ““_°
`the d°5'°°3‘°"-
`weight 1055 8l'3Ph5 W31"3_ PIDW‘-d W_llI1 “SPEC! *0 time-
`51°F“ °r '-hem (°°“'eIa“°“ °°°m°'°m5 °r [hem WI‘-“'5
`larger than 0.997) obtained linear least-square method
`“Sad
`“3 _°aI°“Ia'-3 W313’
`"'3~P°1'
`“3-“5""55i°1''
`(WVTR) "1 the following EcI“ati°n (Chinnan 31- Parks
`1995):
`
`WVTR '-
`
`=
`
`Slope
`Film area
`
`=
`
`g
`11 mi’
`
`where Slope = weight loss vs. time. Film area is the cup
`test mouth area.
`Two WVP values were detemiined by using the
`methods (defined as classical methods throughout the
`study) described by Chinnan and Park (1995) and Ay-
`ranci and Cetin (1995), and corrected method suggested
`by Gennadios, Weller and Gooding (l994a). Eq. (2) was
`used to find WVP in the classical method used as ne-
`
`(R&B cloth thickness tester, James H. Heal, Halifax,
`England) having a sensitivity of 0.001 mm. Films were
`
`glecting gap resistance inside the cup between the solu-
`tion and filrn layer,
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`S. Kayo. A. Kayo I Journal of Food Engineering 43 (2000,! 91' 96
`
`_
`
`93
`
`WVP=
`
`R
`Pt“P1
`
`L.
`
`(2)
`
`(3), calculated p.’ values
`(18 gig mol). From Eq.
`(Table 1) were etnployed in Eq. (2) to calculate the
`corrected WVP.
`
`where WVP is the water vapor permeability, pl the ap-
`parent pressure (kPa) inside the cup, P; the water vapor
`partial pressure (lcPa) at the film outer surface in the
`system. L the average film thickness (mm). The p. and p;
`values were calculated from the product of vapor pres-
`sure of pure water and the relative humidity of the
`medium at
`the defined temperatures and given in
`Table 1. In the classical methods, vapor pressure of
`water inside (p.) the cup were assumed as pure water
`vapor pressure: 0.817, 2.346 and 4.246 kPa, at 4°C, 20°C
`and 30°C. respectively.
`The corrected WVP values were calculated as based
`
`on the reported methods by Gennadios et al. (l994a).
`First of all true pressure (pg) of the film underside was
`calculated.
`
`PI =pr- (pr-po)exp(
`
` ),
`
`prD(MW)
`
`(3)
`
`where pp is the total atmospheric pressure (1 atm), pg
`the partial pressure (atm) of water vapor in air at the
`surface of the solution (or desiccant) in the cup, pl the
`partial pressure (atm) of water vapor at the underside
`of the film. A: the mean stagnant air gap height (m).
`R the gas constant (82.1 x 10" mi’ atrnlg mol K), T
`the absolute temperature (K), D the difiusivity of water
`vapor
`in
`air
`(cmzls)
`found
`in
`the
`literature
`at each temperature, MW the molar weight of water
`
`2.6. Tensile strength, percent elongation, elastic modulus,
`gloss and haze
`
`Mechanical properties were determined using four
`films cast from each solution. Eight strips, 15 cm x 2
`cm, were cut from each type and after conditioning at
`23 :1: 2°C and 45 :1: 5% RH for at least 48 h prior to tests,
`samples were tested for tensile strength and percent
`elongation according to ASTM Standard Method D 882
`(ASTM,
`1993). A TIRATEST 2602 ('1'[RA Ma-
`schinenbau GmbH Raunstein, Germany) was used to
`measure tensile strength, percent elongation and elastic
`modulus of the sample. Initial grip separation and cross-
`head speed were set at 100 and 500 mmlmin, respec-
`tively. The mean of thickness of these films was 0.075
`mm. Haze of samples was measured by using EEL-
`Spherical Hazemeter BS 2782 London, England
`(ASTM, 1970a). Gloss was reported in percentage at 45°
`from a line normal to the surface ASTM, 1970b (n1icro-
`TRI-gloss, BYK-Gardner, Silver Spring, MD). The
`gloss and haze values reported were based on four
`samples and four measurements per sample. These tests
`were applied at room conditions (23 x 2°C and 45 :1: 5%
`RH). It is necessary to test the mechanical properties of
`the films at controlled temperature and relative humidity
`in order to achieve good reproducibility. Since all kinds
`
`Table I
`WVTR. WVP and corrected RI-l (%) values. measured at dillerent temperatures. of 8% and 10% WPI:G film dried using a microwave or room
`conditions (i SD)‘
`
`Drying
`Methods
`
`Microwave“
`
`Room conditions”
`
`Microwave‘
`
`Room conditions‘
`
`Temperature
`(°C)
`
`Thickness
`(mm)
`
`wvra
`tglh 111‘)
`
`RH inside
`Cup ("/o)
`
`WV?
`(g mm! lcPn 11 in‘)
`
`4
`20
`30
`
`4
`20
`30
`
`4
`20
`30
`
`4
`20
`30
`
`0.12
`0.1 l
`0.12
`
`0.1]
`0.10
`0.12
`
`0.10
`0.12
`0.13
`
`0.11
`0.13
`0.13
`
`Classical
`
`Corrected
`
`4.33 (10.1)
`20.33 (10.1)
`40.53 (10.1)
`
`4.85 (10.1)
`20.31 (10.1)
`40.51 ($0.1)
`
`3.11 (10.1)
`9.37 (10.2)
`30.01 (10.1)
`
`3.05 (10.3)
`9.23 (10.2)
`30.55 (10.1)
`
`84 (10.3)
`75 (10.3)
`73 (10.5)
`
`82 ($0.9)
`75 (10.7)
`73 (t|.0)
`
`as (10.9)
`35 (10.7)
`71 (11.1)
`
`39 (10.9)
`57 (10.3)
`75 (10.3)
`
`1 .54 (10. 10)
`1 .90 (10. 10)
`2.35 (10.01)
`
`1.59 ($0.08)
`2.09 ($0.11)
`2.45 ($0.10)
`
`0.97 (10.05)
`1 . 10 (10.01)
`1 .92 (10. 10)
`
`1.09 (10.05)
`1.10 (10.07)
`2.03 (10.10)
`
`2.53 (10.12)
`4.32 (10.13)
`5.40 (10.11)
`
`2.81 (10.14)
`4.70 ($0.12)
`5.65 (10.13)
`
`1.32 (10.12)
`1.51 (10.14)
`3.52 (10.17)
`
`1.49 (10.11)
`1.53 (10.13)
`3.59 (10.20)
`
`‘Thickness are mean values (51) i 0.02). Relative humidity at the inner surface of the film and corrected WVP values were calculated as described by
`Gennadios el al. (1994). RH outside cups was 50%.
`"8% WPI films.
`‘ 10% WPI films.
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`of films were measured at the same room condition, it
`was possible to compare the tensile strength and percent
`elongation of the films.
`
`2.7. Statistical analysis
`
`Sigma Plot V. 3.0 (Jandel Scientific Graphing Soft-
`ware) was used for all statistical analysis. Analysis of
`variance (ANOVA) procedures were used to analyze
`data. Duncan’s Multiple Range Test (p < 0.05) was used
`to detect differences in film property mean values.
`
`3. Results and discussion
`
`3.1. Water vapor permeability
`
`The relative humidity gradient is an important pa-
`rameter in calculation of WVP (MeHugh et al., 1993),
`generally in the literature 100-0%RH (inside—outside the
`cup) was applied (Mel-[ugh et al., 1994; Mate et al.,
`l996).The relative humidity gradient was selected as
`l00—50% since most of the foods have high water ac-
`tivity (>0.95) and environmental RH is generally 50%.
`WVTR values obtained from the slopes of the lines
`(regression eoelficients of the lines were >0.993 at
`p<0.05), obtained from weight loss of cups covered
`with 8% and 10% WPI films prepared with either Ini-
`crowave drying or room conditions, were represented in
`Fig. 1. The increasing WVTR values with increasing
`temperature were observed. It was generally accepted
`that WVTR increased with an increase in temperature
`(Kamper & Fennema, 1984; Gontard, Guilbert & Cuq,
`1993) as it was observed in this study.
`Classical and corrected WVP of the 8% and 10%
`WPI:G films, dried at room conditions or in microwave
`oven. are tabulated in Table 1. It was observed that
`there was no significant dilference between WVP values
`
`of films dried by using these drying methods (p<0.05).
`Classical WVP methods gave lower WVP values than
`calculated values using corrected methods, as it was
`expected, because classical methods ignore air resistance
`between fil.m and solution inside the cup (Gennadios
`et al.,
`l994a). It was found that microwave drying or
`drying at room conditions gave similar results in WVP,
`so it was possible to use a microwave for drying of WPI
`films (Table 1). Mean WVP of 8% WP] films were higher
`than of 10% films, but it was found that there was no
`significant difference in WVP values (p < 0.05). MeHugh
`et al. (1994) reported that there was no significant dif-
`ference in WVP at 8% and 10% WPI:G concentrations.
`
`They used 37.5% sorbitol as plasticizer and 0—l00% RH
`(outlin) and found that WVP values of the WPI films
`(8% and 10%) were the same (2.7lg mm/kPa h m’) and
`they also reported that glycerol addition instead of
`sorbitol increased WVP. The result of this study was in a
`good correlation with their result.
`The WVP values of 8% and 10% WPI:G films, dried
`either in a microwave oven or at room conditions, with
`respect to temperature were given in Fig. 2. Increasing
`WVP with the increasing temperature were observed.
`The different observations were given in the literature
`with the ease of temperature dependency of WVP of
`hydrophilie films, while decrease in WVP with increase
`in temperature was observed for wheat gluten and soy
`protein isolate (Gennadios, Branderburg, Park, Weller
`& Testin,
`l994b),
`increase in WVP with increase in
`temperature was observed for methyl cellulose and hy-
`droitypropyl methyl cellulose films (Chinnan & Park,
`1995).
`
`3.2. Tensile strength, elastic modulus. percent eiangation.
`glass and haze
`
`rapid drying can
`suggested that
`(I986)
`Guilbert
`cause some undesirable mechanical problems such as
`
`3
`
`_ _
`
`I: B9Ht'tvP|:G
`IGWWPEG
`
`or
`
`
`
`
`
`correctedwvecgmmrm’|tPah) 0
`
`so,
`
`— Intvvhlntrn
`
`-
`
`mtsvmlllrn
`
`I
`i.
`
`I
`
`30
`
`
`
`
`
`
`
`Watervaportransntissnonrate{nth-5117}
`
`Temperature (“CI
`
`20
`
`Temperature ("(2)
`
`l. Elleel of temperature on WVTR values of 8% and I0“/o WPl:G
`Fig.
`film dried using microwave (0) or room condition (0).
`
`Fig. 2. Eflcet of temperature on WVP values of 8% and [(1% W'PI:G
`film dried using microwave (0) or room condition (V).
`
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`Table 2
`Some physical properties of films prepared with 8% and l0°/n WPI dried using a microwave or room conditions (1 SD)‘
`
`S. Kayo. A. Kayo I Journal of Food Engineering 43 (2000) 91- 96
`
`Drying methods
`
`Haze
`
`Gloss
`
`Tensile strength
`(MP0)
`
`Modulus of elasticity
`(MPa)
`
`Elongation ("/u)
`
`Microwave“
`Room conditions“
`Microwave"
`Room conditions‘
`
`2.1 (10.2)-
`2.9 (10.1)-
`L8 (10.1)-
`3.2 (10.2)-
`
`9s (12)-
`so (11)-
`9s (12)-
`87 (12)-
`
`2.23 (10.2)--‘-
`L94 (10.2)-
`2.43 (10.1)-
`2.2s (10.3)-J
`
`27.05 (19.5)-
`20.s7 (13.3)-
`20.17 (11.0)-
`l8.9l (15.3)-
`
`36.1(15.3)-
`26.l(;i:2.4)'
`35.9 (14.3)-
`zss (13.1)-
`
`' Numbers with difiercnt following letters differ at P _ 0.05 level.
`* 5% WPI.
`9 10% WPI.
`
`brittleness. However there have been some studies
`
`conducted at higher temperatures rather than at am-
`bient conditions (ca. 23°C). For examples, Kamper and
`Fennema (l984) dried fatty acid and hydroxypropyl
`methylcellulose bilayer films at 90°C for IS min, and
`Gennadios and Weller (1991) dried soymilk protein
`films at 100°C for 1 h. It was planned to dry films by a
`microwave, a rapid dryer, and to control the possible
`increase in brittleness due to rapid drying by knowing
`mechanical properties.
`The tensile strength, percent elongation and elastic
`modulus results were given in Table 2. The 8% and
`10% WPl:G-based films gave similar results, but mi-
`crowave dried films had higher tensile strength and
`elongation values than dried films at room conditions.
`If the results of this study (Table 2) were compared
`with the results given in literature,
`the elongation
`values have been found in the similar range (4.l0"/n
`and 30.8% for WPI:G 5.7:1 and WPI:G 2.3:l, respec-
`tively (McHugh & Krochta,
`l994b)), but the tensile
`strength values of this study were lower than of the
`literature (9.20 and 13.9 MPa for WPl:G 3:] (Fairley
`et al., 1996) and WPI:G 2.3:l (McHugh & Krochta,
`1994b). respectively. Modulus of elasticity is the ratio
`of stress to strain over the linear range and measures
`the intrinsic stillness of the film (Chen,
`I995). Al-
`though the most frequently reported tensile properties
`of edible films are tensile strength and elongation,
`nowadays modulus of elasticity has been given by
`some reporters (Chen, 1995; Fairley cl al., 1996).
`Modulus of elasticity values of WPI films dried using
`microwave or room conditions are given in Table 2. It
`was observed that there was no significant difference
`between modulus of elasticity of the films dried using
`both drying methods. Fairley et al.
`(1996) reported
`in all
`types of edible films, a small
`increase in
`glycerol level results in a large drop in tensile strength
`and an increase in elongation. Their tensile stress.
`elongation and modulus of elasticity (Young's modu-
`lus) were 9.2 MPa, 13.7% and 40! MPa, respectively.
`Since they used WPl:G composition 3:1,
`the lower
`tensile strength and higher elongation values observed
`in this study than their report could be due to the high
`glycerol amount in the solution.
`
`On the other hand, it was known that specular gloss is
`used mainly as a measure of the shiny appearance of
`films and surfaces, and the measurement of haze pro-
`vides some information on the homogeneity of the sur-
`face and internal defects which can contribute to the
`
`the main aim of
`diffusion or deviation of light. So,
`measuring haze and gloss values was to control the
`possible invisible physical degradation of microwave
`drying on films, actually there was not any visible de-
`gradation.
`The gloss and haze of the WPl:G films dried using
`microwave or room conditions, given in Table 2, were
`comparable with the synthetic films, such as gloss
`(measured at 45°) and haze values of the synthetic
`polypropylene films
`(Siiper
`film-Biaxially oriented
`polypropylene film) are 90% and <1.5%, respectively.
`The gloss and haze values of microwave dried films are
`better also than those dried at room temperature. So,
`microwave drying could be applied for drying of WPI
`based edible films.
`
`4. Conclusion
`
`Application of microwave drying to WPI:G based
`edible films did not affect the water vapor permeability
`characteristics. The effect of microwave drying on the
`mechanical properties should be studied in more detail,
`but it was possible to indicate that microwave drying
`could be applied for drying of WPI films. It was im-
`portant to indicate that gloss and haze properties of
`WPI:G based edible films dried by both methods have
`been found as good as the synthetic films.
`
`Acknowledgements
`
`This study was supported by University of Gazia.n-
`tep. Davisco International is greatly acknowledged for
`supplying WPI (BiPro) used throughout this study. The
`authors thank Mr. Necdet Kileci for his help during
`measurements of mechanical parameters of films at
`Siiper Film, Sanko.
`
`RBP_TEVA05022448
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`TEVA EXHIBIT 1017
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`
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`
`TEVA EXHIBIT 1017
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
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`RBP_TEVA05022449
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`TEVA EXHIBIT 1017
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC