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MEASUREMENT OF FIRMNESS OF STIRRED YOGURT IN ROUTINE QUALITY CONTROL

GASTN ARES1, CAROLINA PAROLI3 and FEDERICO HARTE2,4


1

Seccin Evaluacin Sensorial Facultad de Qumica

Unidad de Tecnologa de Alimentos Facultad de Agronoma Universidad de la Repblica Montevideo, Uruguay


3

Carrera Ingeniera de Alimentos Universidad de la Repblica Montevideo, Uruguay

ABSTRACT The objectives of the present work were to evaluate the potential use of the vane method and penetration tests as a tool to measure the variability in rmness of stirred yogurt in routine quality control, and to evaluate the effect of distribution on yogurt rmness. Twelve batches of plain stirred yogurt of a commercial brand were studied, acquired both from a manufacturing plant and three retail stores. Both vane method and penetration tests allowed the detection of changes in the rmness of yogurts, conrming that they could be useful in routine quality control to characterize the rmness of yogurt. The yield stress of samples from the manufacturing plant varied within a range of 250 Pa. This important variation was partially explained by variations in the nal acidity during fermentation, showing the importance of a standardized production in order to obtain a uniform texture. The yield stress of yogurts from the manufacturing plant was signicantly higher than that of samples from the different retail stores. Averaged values being considered, the yogurts lost 53 Pa of their original yield stress during distribution and handling inside retail stores, probably due to mechanical damage. This mechanical damage also caused the occurrence of syneresis.

Corresponding author. Department of Food Science and Technology, The University of Tennessee, 2509 River Drive, Knoxville, TN 37996. TEL: 865-974-7265; FAX: 865-974-7332; EMAIL: fede@utk.edu Journal of Food Quality 29 (2006) 628642. All Rights Reserved. 2006, The Author(s) Journal compilation 2006, Blackwell Publishing

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INTRODUCTION Texture is one of the main characteristics that dene the quality of yogurt and affect its appearance, mouthfeel and overall acceptability (Kroger 1975; Yoon and McCarthy 2002). The most frequent defects related to yogurt texture, which may lead to consumer rejection, are apparent viscosity variations and the occurrence of syneresis (Kroger 1975; Keogh and OKennedy 1998). The maintenance of a uniform texture and particularly rmness among different units, processing dates and shelf life is a prime goal in yogurt production (Chanasattru et al. 2002). Yogurt texture may vary due to variations in milk composition, as well as changes in processing, incubation and storage conditions (Tamime and Deeth 1980). Stirred yogurt might also suffer changes in its texture due to mechanical damage during distribution (Ramaswamy and Basak 1992). However, no studies have been found reporting the effect of distribution on yogurt rmness. Yogurt is a non-Newtonian pseudoplastic material, with a highly timedependent behavior (Basak and Ramaswamy 1994; Benezech and Maingonnat 1994). Measuring its rheological behavior is difcult because of its poor reproducibility, sensitivity to sample preparation, sensitivity to shear history and wall slip (Yoon and McCarthy 2002). These problems make rheological characterization a challenge in routine quality control, where many samples are determined in short time frames. Apparent viscosity is usually a standard routine measurement in the yogurt industry. However, as apparent viscosity decreases irreversibly as a function of shear rate and time, placing yogurt into the narrow gap of a viscometer produces an important disruption of its structure (Suwonsichon and Peleg 1999). Therefore, highly standardized procedures are required in order to obtain reproducible results. Empirical or imitative methods such as penetrometry tests, texture prole analysis and Posthumus funnel have been preferred to characterize the textural properties of yogurts (Hellinga et al. 1986; Dave and Shah 1998; Fiszman and Salvador 1999; Fiszman et al. 1999; Haque et al. 2001). Penetration tests constitute one of the simplest and most widely used types of texture-measuring methods. They are inexpensive, can be generally correlated to sensory measurements and do not require mathematical treatments (Benezech and Maingonnat 1994). The main disadvantages of these empirical methods, when compared to fundamental measurement of rheological properties, are the use of relative scales and that results are for a given set of experimental conditions, making it hardly possible to compare results unless the same conditions are used (Benezech and Maingonnat 1994). Yield stress, a rheological property dened as the minimum shear stress required to initiate ow, can be used to characterize the rmness of yogurt.

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Yield stress is not easy to measure because its magnitude depends on the characteristic time of the sample, the characteristic time of the process, as well as on the history of structural alteration of the sample prior to measurement (Cheng 1986; James et al. 1987; Genovese and Rao 2003). Many indirect and direct methods have been suggested for the measurement of yield stress (Nguyen and Boger 1985; Yoshimura and PrudHomme 1987; Steffe 1996). The vane method has been used to determine the yield stress of many dairy foods including yogurt (Jaar 1998; Harte et al. 2003b), ice cream (Briggs et al. 1996), cream cheese (Breidinger and Steffe 2001) and sour cream (Daubert et al. 1998). According to Harte et al. (2003a), the vane yield stress of yogurt is highly correlated with the sensory rmness evaluated by trained panelists. The vane method has a potential use in quality control as it allows a simple, objective and direct determination of yield stress with no structural damage prior to measurement (Nguyen and Boger 1985; James et al. 1987). The objectives of the present work were to: (1) evaluate the potential use of the vane method and penetration tests as a tool to measure the variability in rmness of stirred yogurt in routine quality control, both in the manufacturing plant and retail stores; (2) correlate the variation in yogurt rmness with compositional and production parameters; and (3) evaluate the effect of distribution on the rmness of stirred yogurt.

MATERIALS AND METHODS Samples Small jars of plain stirred yogurt (200 mL) of a commercial brand were studied. According to the information provided by the manufacturer, the ingredients used in the products manufacture were pasteurized milk, sugar, skimmed powdered milk, sodium caseinate, yogurt culture, modied starch and gelatin. Twelve batches were studied during a period of 3 months. Samples from the same batch were acquired from four different places: manufacturing plant and three local retail stores, selected according to their distance to the manufacturing plant: RS1 (5 km), RS2 (10 km) and RS3 (25 km). Four samples of each batch were acquired directly from the manufacturing plant, and two samples from the same batch were acquired at each retail store. The samples were stored in their original retail containers approximately 72 h at 5 1C before texture and chemical determinations.

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Vane Yield Stress Determination Yield stress determinations were performed on samples in their original retail containers, using a Haake VT500 coaxial viscometer (Haake MessTechnik, Karlsruhe, Germany) equipped with a four-blade vane geometry (12.67 mm in diameter, 25.35 mm in height). The vane was gently fully immersed in the sample, with its top surface even with the sample surface. It was rotated at a constant speed of 2 rpm for 90 s. The torque required to maintain this motion was recorded as a function of time using VT500/501 Software v.1.7 (Haake Mess-Technik). Yield stress was calculated using the peak value of torque using the following equation (Steffe 1996):

2M H 1 = + 3 Dv 3 Dv

where t is the stress, M is the torque, Dv is the vane diameter and H is the vane height. The sample and geometry were kept at 5C until each determination. Duplicate measures for each batch and place were performed. Penetration Tests After yield stress determination, penetration tests were performed on samples in their original retail containers, with a TA.XT2 Texture Analyzer (Stable Micro Systems, Godalming, U.K.), using a 12.7-mm at-end Perspex cylindrical probe. Force and time data were recorded using the Texture Expert Software (version 1.0) from Stable Micro Systems. Samples were penetrated 20 mm. The speed of the probe was 1.0 mm/s during the pretest, penetration and relaxation. The trigger force was 1 g. Duplicate measures for each batch and place were performed. From the force-versus-time curves, values for the following textural parameters were calculated (Fig. 1): force at a distance of 0 mm (F0), force at a distance of 4 mm (F4 mm), slope of the linear part of the compression curve (slope), force at a distance of 20 mm (F20 mm), rst part of the curve (slope), force and distance at which a deviation from linear behavior of the compression curve was observed (Fl and dl, respectively). Syneresis In order to measure the syneresis that occurred during storage of the yogurts, the serum present in the surface of the samples was extracted and measured using a syringe (Fiszman et al. 1999).

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F20

Fl

slope
Force (N)

F0

4 mm

dl

Distance (mm)

20 mm

FIG. 1. TYPICAL FORCE-VERSUS-DISTANCE CURVE FROM PENETRATION TESTS SHOWING THE PARAMETERS THAT WERE CALCULATED FROM THE CURVE Force at a distance of 0 mm (F0), force at a distance of 4 mm (F4 mm), slope of the linear part of the compression curve (slope), force at a distance of 20 mm (F20 mm), rst part of the curve (slope), force (Fl) and distance (dl) at which a deviation from linear behavior of the compression curve was observed.

Composition Ash, fat (AOAC 1995), protein (FIL-IDF 20 1962) and total solids content (FIL-IDF 151 1991) of each sample were determined by standard techniques. Carbohydrate content was determined as the difference between total solids, fat, ash and protein content. The pH of each sample was determined by measurement on the day of texture evaluation using a pH meter (Cole Parmer, Vernon Hills, IL). Data Analysis Results were analyzed as a factorial experiment in a completely randomized design. Analysis of variance (ANOVA) was performed for the variables yield stress and penetration parameters, considering the batch (manufacturing

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date) and place of purchase as variation factors. Least signicant differences were calculated by the Fishers test. Differences were considered signicant when P 0.05. The coefcient of variation of yield stress between samples for each place of purchase was calculated using the error mean square from ANOVA and the mean value of yield stress for that place of purchase (n = 28). The coefcient of variation of yield stress between batches for each place of purchase was calculated using the mean values of yield stress for each batch and calculating the mean and SD of those values (n = 28). In order to evaluate the effect of mechanical damage during the distribution and handling of yogurts inside the retail stores, a t-test for the comparison of linkage means was carried out on the yield stress data obtained for yogurts from the manufacturing plant and retail stores (a = 0.05). A principal component analysis (PCA) of the mean rating for yield stress and penetration tests data was used to illustrate the relationship among the different texture parameters. Linear partial least squares (PLS) regression analysis was used to analyze the relationships between yield stress and compositional and production data matrices (Martens and Martens 1986). PLS regression is a modeling approach commonly used when predictive variables are intercorrelated. It proceeds by extracting a few linear combinations (PLS factors) of the response data that predict as much of the variations in the predictive data as possible. To ensure an accurate prediction of responses, PLS constructs several submodels to establish the strongest association between these factors (Martens and Martens 1986). Ostens F-test was used to determine the number of signicant (P < 0.05) factors. This test compares cross-validation sum of squares from the current dimension with the change of cross-validation sum of squares from the previous dimension. XLSTAT version 7.5.3 statistical software (Addinsoft, New York, NY) was used for all these analyses.

RESULTS AND DISCUSIN Vane Yield Stress Determination Yield stress values for plain stirred yogurts ranged from 20 to 400 Pa, depending on the batch and the place of the sample. These values are higher than those reported by Ramaswamy and Basak (1991, 1992), Benezech and Maingonnat (1993) and Harte et al. (2002). The difference might be due to the fact that these authors determined the yield stress using methods that caused an extensive structural damage prior to measurements (extrapolation from ow

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4 0 0 ,0

3 5 0 ,0

3 0 0 ,0

2 5 0 ,0

Yield stress (Pa)

2 0 0 ,0

M a n u fa c tu rin g p la n t R e ta il S to re 1

1 5 0 ,0

R e ta il S to re 2 R e ta il S to re 3

1 0 0 ,0

5 0 ,0

0 ,0 0 2 4 6 8 10 12

B a tc h

FIG. 2. YIELD STRESS OF THE DIFFERENT BATCHES, FOR YOGURTS OBTAINED IN THE MANUFACTURING PLANT AND IN RETAIL STORES Mean SD.

curves to zero shear rate [Ramaswamy and Basak 1991, 1992; Benezech and Maingonnat 1993], and determination of the shear stress at which ow rst begins [Harte et al. 2002]). However, the values obtained in the present study are in agreement with those reported by Jaar (1998), who used the vane method at a constant rotational speed of 1 rpm to determine the yield stress of stirred yogurt. The coefcient of variation among units from the same batch and place of purchase was low, with a maximum of 8.8%. This indicates the high reproducibility of vane yield stress determination. ANOVA showed that the vane method signicantly detected (P < 0.001) changes in rmness of yogurt from different batches and places of purchase. An important variation in yield stress between the different batches was observed. As shown in Fig. 2, important oscillations were recorded in the yield stress of the yogurts obtained directly from the manufacturer. This variation can be illustrated by the coefcient of variation between samples calculated using the mean values of yield stress obtained for each batch. As shown in Table 1, the variation coefcient reached 28.7% for the samples obtained from different processing dates and the same manufacturer. Moreover, the range (calculated as the difference between the maximum and the minimum yield stress value) shows that yield stress varied in a range of nearly 250 Pa

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TABLE 1. COEFFICIENT OF VARIATION BETWEEN SAMPLES AND BETWEEN BATCHES AND RANGE FOR THE VANE YIELD STRESS OF SAMPLES FROM THE MANUFACTURING PLANT AND DIFFERENT RETAIL STORES Place Coefcient of variation between samples (%) 5.6 8.8 8.0 5.1 Coefcient of variation between batches (%) 28.7 36.0 32.8 34.4 Range (Pa)

Manufacturing plant Retail store 1 Retail store 2 Retail store 3

249.85 249.85 195.70 267.87

(Table 1). According to Harte et al. (2006), a panel of ve trained sensory assessors is able to detect differences of approximately 50 Pa in yield stress of stirred yogurt. Therefore, as in this case, the range was nearly ve times greater than the minimum difference that a sensory panel can detect; the observed variation might be perceived by consumers. These results showed that yogurts from the manufacturing plant did not have a constant rmness, and therefore, a routine control of this parameter was suggested. Signicant differences in yield stress were found between those samples from the manufacturing plant and from the different retail stores. Averaged values being considered, the yogurts lost 53 Pa of their original yield stress during distribution and handling inside the retail stores. The yield stress of the yogurt samples from the manufacturer was signicantly higher than that of samples from the retail stores. These results show that mechanical damage during yogurt distribution and in the retail stores causes a decrease in the rmness of yogurt. These differences were, in many cases, masked by the fact that a loss of 123-Pa yield stress was found for batches from the same manufacturer and different dates. The average and maximum differences between yield stress of samples from the manufacturing plant and those from the retail stores were calculated for each retail store. The highest average difference (P < 0.05) was found in retail store 2 (46.1 Pa), followed by retail stores 1 and 3 (30.5 and 36.5 Pa, respectively). Moreover, the maximum difference was also found in retail store 2 (123.5 Pa) followed by retail stores 1 and 3 (84.5 and 79.4 Pa, respectively). These results showed that the higher mechanical damages were not found in retail store 3, which was the farthest retail store from the manufacturing plant. Therefore, the loss in yield stress was not correlated to the distance from the manufacturing plant to the retail store, suggesting that yogurt manipulation inside the retail stores was the main cause of mechanical damage to yogurt.

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This mechanical damage during distribution and handling inside the retail stores also caused the occurrence of syneresis. While none of the samples from the manufacturing showed syneresis, some batches from the retail stores showed the occurrence of syneresis (values ranging from 0.2 to 1 mL). Syneresis was found in two batches from retail stores 1 and 3, and in four batches from retail store 2. This also suggests that yogurts in retail store 2 suffered the higher mechanical damage. Relationship between Yield Stress Variations and Composition and Production Data Changes in the composition of yogurts, as well as changes in the production process, may have promoted the registered variations in the yield stress of the different yogurt batches. Signicant (P < 0.001) changes in all the evaluated compositional parameters were observed for the different batches considered. Protein content varied within a range of 0.4%, fat content within a range of 1.5%, while pH within a range of pH 0.2. These variations are known to cause changes in the rmness of yogurt (Jaar 1998; Beal et al. 1999). Furthermore, because the manufacturer did not use a xed criterion to determine the end of the fermentation process, both fermentation time and nal acidity were variable. The nal acidity at which fermentation was stopped for each of the considered batches varied within a range of 8D, causing variations in the texture of yogurt (Beal et al. 1999). A PLS regression was performed in order to identify the relationship between the variation of yield stress and the variation of the evaluated parameters of composition and production of the different batches of yogurt. Yield stress was considered the response variable and the evaluated parameters of composition and production the independent variables (pH, protein, fat, carbohydrates, total solids and nal acidity). Leverage-corrected residuals showed optimal prediction ability for the two PLS regression factors, explaining 59.8% of the total variance of Y. The rst PLS dimension explained 53.8% of the variance of the compositional and production data and 36.4% of the variance of the yield stress data; whereas the second PLS dimension explained 24.5 and 23.4% of the compositional and yield stress data, respectively. Ostens F-test determined that factors 1 and 2 were valid predictors (P < 0.05). Figure 3 shows that yield stress was positively correlated to nal acidity. With the regression coefcients for the evaluated chemical and production data being considered, the only signicant coefcient was that related to nal acidity (0.791). This regression suggests that part of the variation in yield stress was due to the variation in nal acidity, whereas it

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1 0,75 Yield stress Final acidity 0,5 0,25 0 -0,25 -0,5 -0,75 -1 -1 -0,75 -0,5 -0,25 0 0,25 0,5 0,75 1 Fat pH Protein Carbohydrates Total solids

PLS2 (23.4%X, 24.5%Y)

PLS1 (53.8% X, 36.4% Y)


FIG. 3. CORRELATION COEFFICIENTS OF PARTIAL LEAST SQUARES (PLS) YIELD STRESS VALUES VERSUS COMPOSITIONAL AND PRODUCTION DATA

was not explained by the variation in the composition of yogurts. Not all the variation in yield stress was explained by the evaluated parameters, suggesting that other production parameters might be responsible for the important variation observed.

Penetration Tests Typical force-versus-distance (N mm) curves are shown in Fig. 1, similar to those obtained by Fiszman and Salvador (1999). The curves were remarkably reproducible and enabled characterization of the samples in terms of the various parameters evaluated (F4 mm, slope, F20 mm, Fl and dl). The coefcient of variation among units from the same batch and place of purchase was lower than 10% for all parameters, showing the high reproducibility of penetration tests. The mean values obtained throughout the study are shown in Table 2. ANOVA showed a highly signicant effect of the batch and retail store on all the evaluated parameters, which indicates the validity of penetration tests to detect changes in the texture of yogurt.

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TABLE 2. AVERAGE VALUES OF TEXTURE PARAMETERS OBTAINED DURING PENETRATION TESTS FOR SAMPLES OBTAINED IN THE MANUFACTURING PLANT AND RETAIL STORES (MEAN SD) F4 mm (N) 0.110 0.003 0.107 0.005 0.099 0.003 0.099 0.003 0.0181 0.0002 0.0162 0.0003 0.0143 0.0002 0.0139 0.0002 0.203 0.002 0.201 0.003 0.185 0.002 0.184 0.002 Slope (N/mm) F20 mm (N) Fl (N) 0.165 0.002 0.150 0.004 0.136 0.003 0.138 0.003 dl (mm) 7.00 0.05 6.80 0.07 6.20 0.07 6.30 0.07

Place

F0 (N)

G. ARES, C. PAROLI and F. HARTE

Manufacturing plant Retail store 1 Retail store 2 Retail store 3

0.041 0.003 0.044 0.004 0.045 0.003 0.045 0.003

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1 Fo

0,5

-- PC2 (13,20 %) -->

F4mm 0 slope F20mm Fl Yield stress dl

-0,5

-1 -1 -0,5 0 0,5 1

-- PC1 (72,91 %) -->

FIG. 4. FACTOR LOADINGS OF THE PRINCIPAL COMPONENT ANALYSIS (PCA) OF THE INSTRUMENTAL TEXTURE DATA

PCA The correlation matrix of the instrumental data showed that yield stress was positively correlated with F4 mm, slope, F20 mm, Fl and dl (r 2 higher than 0.89). Although Fiszman and Salvador (1999) mentioned that the force at the nal distance of a penetration test was not related to any physical characteristic of yogurt, it was found to be highly correlated to vane yield stress. PCA was performed in order to visualize the relationship between the evaluated parameters. The rst two principal components accounted for 72.9 and 13.2% of the variance, respectively, in the PCA of the instrumental texture data for all the yogurt samples (Fig. 4). The rst principal component was positively correlated with yield stress, F4 mm, slope, F20 mm, Fl and dl. Therefore, a higher loading in PC1 means a higher rmness in yogurt. The second component was dened positively with F0. This parameter has not been reported to be related to any textural characteristic. These results suggest that both methods give similar results and that both could be used to characterize the rmness of stirred yogurt. Moreover, except for F0, all the other parameters from the penetration test were correlated to each other, which indicates that the number of parameters could be reduced in routine analysis.

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CONCLUSIONS Both vane method and penetration tests allowed the detection of changes in the rmness of yogurts. These determinations were performed on samples in their original retail containers, using quick and direct techniques that could avoid the use of time-consuming, highly standardized procedures. Therefore, both methods could be useful in routine quality control to characterize the rmness of yogurt. The yield stress of the samples from the manufacturing plant varied within a range of 250 Pa. This important variation, which might be perceived by consumers, was partly explained by changes in the nal acidity during fermentation, showing the importance of a standardized production in order to obtain a uniform texture. The yield stress of yogurts from the manufacturing plant was signicantly higher than that of samples from the different retail stores. The loss in yield stress was not correlated to the distance from the manufacturing plant to the retail store, suggesting that yogurt manipulation inside the retail stores was the main cause of mechanical damage to yogurt. This mechanical damage also caused the occurrence of syneresis. REFERENCES AOAC. 1995. Ofcial Methods of Analysis, 16th Ed., Vol II, AOAC International, Gaithersburg, MD. BASAK, S. and RAMASWAMY, H.S.A. 1994. Simultaneous evaluation of shear rate and time dependency of stirred yogurt rheology as inuenced by added pectin and strawberry concentrate. J. Food Eng. 21(3), 385393. BEAL, C., SKOKANOVA, J., MARTN, N. and CORRIEU, G. 1999. Combined effects of culture conditions and storage time on acidication and viscosity of stirred yogurt. J. Dairy Sci. 82(4), 673682. BENEZECH, T. and MAINGONNAT, J.F.A. 1993. Flow properties of stirred yoghurt: Structural parameter approach in describing time-dependency. J. Texture Studies 24(4), 455473. BENEZECH, T. and MAINGONNAT, J.F.A. 1994. Characterization of the rheological properties of yoghurt. J. Food Eng. 21(4), 447472. BREIDINGER, S.L. and STEFFE, J.F. 2001. Texture map of cream cheese. J. Food Sci. 66(3), 453457. BRIGGS, J.L., STEFFE, J.F. and USTANOL, Z. 1996. Using the vane method to evaluate the yield stress of frozen ice cream. J. Dairy Sci. 79, 527531. CHANASATTRU, W., CORRADINI, M.G. and PELEG, M. 2002. Determination of practically signicant differences in the sensorily perceived consistency of semiliquid foods. J. Texture Studies 33(5), 445460.

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