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Journal of Food Engineering 87 (2008) 303–313 www.elsevier.com/locate/jfoodeng

Review

Near infrared spectroscopy for on/in-line monitoring of quality in foods and beverages: A review
Haibo Huang, Haiyan Yu, Huirong Xu, Yibin Ying *
College of Biosystems Engineering and Food Science, Zhejiang University, 268 Kaixuan Road, Hangzhou 310029, China Received 17 June 2007; received in revised form 17 December 2007; accepted 22 December 2007 Available online 8 January 2008

Abstract Over the past 30 years, on/in-line near infrared (NIR) spectroscopy has proved to be one of the most efficient and advanced tools for continuous monitoring and controlling of process and product quality in food processing industry. A lot of work has been done in this area. This review focuses on the use of NIR spectroscopy for the on/in-line analysis of foods such as meat, fruit, grain, dairy products, beverage and other areas, and mainly looks at the literature published in the last 10 years. The topics covered emphasize the methods designed for on/in-line measurement of data, chemometric treatment, as well as interpretation of the experimental observations. Finally, problems relating to the successful applications of on/in-line NIR spectroscopy in production processes have been briefly outlined. Ó 2008 Elsevier Ltd. All rights reserved.
Keywords: Near infrared spectroscopy; Foods and beverages; Quality; On/in-line; Process monitoring

Contents 1. 2. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1.1. NIR spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Applications in food systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.1. Meat . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.2. Fruits and vegetables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.3. Grain and grain products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.4. Dairy products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.5. Oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.6. Fish and fish products . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.7. Beverages . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.8. Others . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.9. Constraints of NIR techniques in food analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.10. Conclusions and future outlook . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Acknowledgements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 304 304 304 304 305 307 308 309 309 310 310 310 310 311 311

*

Corresponding author. Tel.: +86 571 86971140; fax: +86 571 86971885. E-mail address: ybying@zju.edu.cn (Y. Ying).

0260-8774/$ - see front matter Ó 2008 Elsevier Ltd. All rights reserved. doi:10.1016/j.jfoodeng.2007.12.022

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1. Introduction During the last 50 years, there has been a lot of emphasis on the quality and safety of the food products, of the production processes, and the relationship between the two (Burns and Ciurczak, 2001). These requirements call for on-line detection techniques which have the following advantages: (i) can be assembled in the production line and take place under realistic environment, (ii) early detection of possible failures, (iii) permanent monitoring of the conditions, (iv) assessment of conditions at any desired time (Pemen et al., 1998). These advantages enable detection of quality changes of raw materials and final product under steady process conditions Compared to other nondestructive techniques, NIR spectroscopy does not need any sample preparation. Hence the analysis is very simple and rapid, which is a requirement for on-line application. Furthermore, NIR technique allows several constituents to be measured simultaneously. Finally, the relatively weak absorption due to water enables high-moisture foods to be analyzed (Osborne, 2000). All these properties make NIR technique widely acceptable in recent years as one of most promising on/in line detection methods in food and other areas. Industries involved with foods and beverages have traditionally used NIR measurements for quality control, blending, and process control (Workman et al., 1999). Developments in computer science and chemometrics have prompted parallel developments in the on/in-line NIR techniques, and have attracted considerable attention from food researchers. For example, this technique was applied for on-line detecting fat, moisture, and protein content during meat processing (Isaksson et al., 1996). With respect to grains, some researchers have installed NIRS equipment in the harvester for continuous detection of parameters characterizing grain quality such as protein and moisture content (Maertens et al., 2004). These on/in-line applications have established their control capability in food processing. 1.1. NIR spectroscopy NIR spectroscopy is based on the absorption of electromagnetic radiation at wavelengths in the range 780– 2500 nm. NIR spectra of foods comprise broad bands arising from overlapping absorptions corresponding mainly to overtones and combinations of vibrational modes involving C–H, O–H, and N–H chemical bonds (Osborne, 2000). This makes it very feasible for measurements to be made in organic and biological systems. Radiation interacting with a sample may be absorbed, transmitted or reflected. Thus, there are different NIR spectroscopy measurement modes fitting different applications. In practice, the common modes are transmittance, interactance, transflectance, diffuse transmittance, and diffuse reflectance, with the last two being most frequently used. Diffuse transmittance measurements are usually carried out in the region of the spectrum between 800 and 1100 nm where

Fig. 1. Illustration of an on-line NIR instrument with the MM55 gauge mounted at the outlet of a meat grinder (Isaksson et al., 1996).

weak absorptions enable useful data to be obtained using sample thickness of 1–2 cm, such as with meat, cheese or whole grain. In the wavelength range 1100–2500 nm, the amount of scattering makes the path length so high that transmittance through 1 cm thickness of most samples is negligible. This situation is called diffuse reflectance because most of the incident radiation is reflected. This measurement is suitable for thicker samples such as fruits and wheat power. 2. Applications in food systems 2.1. Meat Meats are very susceptible to spoilage and are also expensive as compared to other food types. Hence, there has been a considerable interest in measuring their composition and quality, in order to improve the efficiency of unit operations applied in meat processing (Hildrum et al., 2004). From an industrial and marketing perspective, the major raw materials in the processing of meat are carcasses of beef and pork. NIR analysis is capable of rapid assessment of fat, water, protein, and other parameters simultaneously (Clark and Short, 1994; Hildrum et al., 1994; Isaksson et al., 1995; Alomar et al., 2003; Geesink et al., 2003; Prevolnik et al., 2005; Prieto et al., 2006; Savenije et al., 2006). However, NIR technique had not been used for on/in-line detections of meat until 1996. The first on-line application of this technique was reported for determination of fat, moisture, and protein contents in ground beef (Isaksson et al., 1996) on a conveyor using a diffuse NIR instrument set at the outlet of the meat grinder (Fig. 1), using multiple linear regression (MLR) as the calibration method. Besides being feasible for on-line determination of parameters of meat quality, the amount of sample required was relatively small. Tøgersen

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et al. (1999) extrapolated this concept to determine fat, water, and protein content in beef and pork in industrial scale batches. Although the amount of sample was much larger than that reported by Isaksson et al. (1996), the prediction errors were similar. Thereafter, with the same equipment by reflectance spectroscopy, TØgersen et al. (2003) determined fat, water, and protein content in semifrozen raw meat, which is largely used in the manufacturing industry, due to mismatches between supply and demand of raw meat in the market. A NIR reflectance instrument with a diode array detector was applied for in-line monitoring of the proximal composition of ground beef on a conveyer belt. (Hildrum et al., 2004). This technique makes it possible to perform measurements over large meat surface areas on each batch under industrial conditions. Sixty batches of coarsely ground beef were processed under industry conditions and monitored continuously. After removing signals originating from the belt itself, the remaining data were used to form partial least squares (PLS) models for each component in beef at two different sizes. The results showed that the predictions were generally better when using smaller grinding size. In addition, a forward variable selection method based on jack-knifing was used, and obtained similar results. A NIR transmission system for on-line measurement of fat in unhomogenized meat has been reported by Schwarze (1997). The system was used for the continuous analysis of meat products with varying composition and particle size during mixing process. Samples were automatically extracted, analyzed and fed back into mixer. The results showed NIR spectroscopy to be suitable for on-line monitoring fat contents during meat processing. Modern blending operations use two blending steps to achieve a target fat content, whereas only one step would be required if the fat content of the unblended heterogeneous stream of ground beef were determined on-line. With the purpose of eliminating blending steps and improving the quality of blended beef, Anderson and Walker (2003a) applied the Perten DA700 NIR/VIS analysis system for measuring fat content in ground beef in the moving stream of meat formed by a grinder equipped with a custom forming head. The measurements on 27 kg blocks of beef achieved high accuracy with SEP (Standard Error of Prediction) of 1.00–1.68% for the calibration set and 2.15–2.28% for the validation set. However, it did not show how or whether these measurements could effectively eliminate a blending step. Thus, thereafter, a simulation was used by Anderson and Walker (2003b) to demonstrate the efficacy of on-line visible/near infrared spectroscopic measurements of fat content in the streams of ground beef to achieve a target fat content in a final blender. Three styles of control limits (constant limit, tapered limit, and funnel limit) were tested for the model, which was calibrated by more than 10,000 spectra from 31 blocks of frozen beef. The control limits for these styles achieved the target fat content with a tolerance of 0.75% fat, 99.7% of the time.

On-line analysis of fatty acids (C14:0, C16:0, C16:1, P C17:0, C17:1, C18:0, C18:1, C18:2, C18:3, and polyunP P saturated, monounsaturated and saturated) in the intramuscular and subcutaneous fat in Iberian pork loin has been successfully achieved using NIR spectrometer equipped with a remote reflectance fiber-optic probe (Gon´ ´ zalez-Martın et al., 2003, 2005). In addition to predicting chemical parameters, visible and NIR spectroscopy was also used for on-line analysis of tenderness of longissimus steaks during commercial beef carcass grading (Shackelford et al., 2004). Interference by signals caused by uneven surface of moving meat poses a serious problem during on-line monitoring of ground beef composition on a conveyor belt using a NIR reflectance sensor. Thus, no good calibration models were obtained with the original raw spectra. Westad et al. (2004) developed a soft independent modeling of class analogies (SIMCA) classification method for yielding pure meat spectra, which was shown to be useful. NIR spectroscopy could also used to determine sodium chloride (NaCl) in cured meat. As early as 1984, Begley et al. (1984) applied the NIR technique to measure the amount of NaCl in canned cured hams. A high correlation between salt content determined by chemical analysis and by NIR spectra at 1806 nm was obtained. Finally, they concluded that the ability of NIR to measure salt content was due to a shift in the water spectrum caused by saltinduced changes in the amount of hydrogen bonding. 2.2. Fruits and vegetables Fruit and vegetables are a unique class of food items in a sense that their size, colour, shape, and chemical composition vary, even when harvested at the same place and same time. Hence, sorting them on the basis of their quality is very important. Use of conventional analytical techniques is very time-consuming and labour intensive. NIR spectroscopy is an attractive non-destructive technology well-suited to the measurement of moisture in fruit and vegetables (Kays, 1999). Determination of quality parameters under off-line conditions using NIR instrumentation has been reported previously (Slaughter et al., 1996; Shen et al., 1998; Hart et al., 1998; Lu, 2001; Terasaki et al., 2001; ´ Liu and Ying, 2004; Walsh et al., 2004; Gomez et al., 2006), providing an impetus for the development of on-line monitoring and grading techniques. Kawano et al. (1992, 1993) used NIR spectroscopy for determination of sugar content in intact peaches and mandarins, and reported an automated fruit sorting machine based on this principle. Since then, on-line NIR has been widely applied in fruit and vegetable processing. Choi (1998) developed an on-line machine based on NIR reflectance spectroscopy for real time determination of sugar content at a sorting speed of two fruits per second. A good result with a low SEP of 0.78 °Brix was obtained in Fuji apples; such errors were acceptable for rapid on-line detection. High-resolution laboratory-based spectrometers are

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commercially available, but are generally expensive and not feasible for on-line integration in an industrial process. Greensill and Newman (2001) reported the performance of three simple wavelength dispersion elements (single equilateral prism, two equilateral prisms in series, and ruled diffraction grating) for the design of a simple, low-cost, and robust NIR spectrometer for application in automated fruit grading systems. They found all the designs to perform well; the dual-prism instrument demonstrated the highest potential for reliable, rapid sorting of the fruit than the other two types. He et al. (2001) compared three NIR measuring methods: the on-line reflex, the partially shaded light transmission and the fully shaded light transmission. They detected sugar content, acidity, and internal browning in oranges and apples by a fully shaded light transmission detecting device. Satisfactory results were obtained with R2 of 0.95 for °Brix, and 0.85 for acidity. Both the on-line commercial NIR equipment and hand-held NIR units were used to measure °Brix level of Florida citrus by Miller and Zude (2002). For the determination, spectral data were obtained using two light sources mounted on a special cup, placed against the fruit’s surface. The on-line tests were conducted at a rate of 5.5 fruits per second. For calibration, linear regression relationships were developed between the non-destructive NIR techniques and the labo-

ratory Brix measurements. However, all R2 values were lower than 0.7. Then, they evaluated a neural network model with combined inputs of physical and colour attributes and predicted °Brix using NIR. Correct classification accuracy was $90% for 10°Brix, and $80% for 11°Brix set point. Internal browning is a disorder that affects many varieties of commercial apple cultivars including ‘Braeburn’, ‘Sunrise’, ‘Fuji’, ‘Red Delicious’ and ‘Golden Delicious’ (Elgar et al., 1999; Lau and Lane, 1998; Volz et al., 1998; Keener et al., 1999). Hence, development of accurate non-destructive test methods for on-line inspecting of fruits for internal browning and removing them from consignments is a long-felt necessity. Clark et al. (2003) appraised the use of NIR transmittance to segregate ‘Braeburn’ apples affected by a full range of browning, by applying different analytical techniques to fruit in different orientations, and concluded it to be suitable for sorting fruits, and thereby reduce the incidence of ‘Brownheart’ in commercial consignments. Thereafter, practical prototype systems were constructed and tested (McGlone et al., 2005). These systems demonstrated an accurate measurement of ‘Brownheart’ in fruits moving at realistic grading speeds. Two specific on-line transmission systems (a time-delayed integrating spectrometer (TDIS), and a large aperture spectrometer (LAS) (Fig. 2) were constructed and compared.

Fig. 2. A conceptual view of NIR transmission system. As the fruit passes through a relatively large field-of-view in the TDIS system (A), a detector simultaneously accumulates many sequential points over three apples. In contrast, the LAS system (B) takes a simple snapshot, like a camera, over a much shorter time for a small portion of one fruit (McGlone and Martinsen, 2004).

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These two systems were each optimally configured to operate at typical grader speeds (500 mm sÀ1 or approximately five fruit per second), and detect the low levels of light diffusely transmitted through apples in the wavelength range 650–950 nm. Finally, they concluded LAS system to give better results. In addition, these two systems were previously tested by McGlone and Martinsen (2004) for their ability to measure dry matter (DM) in apples. Both these gave excellent predictions with standard errors of less than 0.5% at the speed of 500 mm sÀ1. NIRS technique was used by Golic and Walsh (2006) to sort stone fruits (peaches, nectarines, and plums) on the basis of total soluble solids in an in-line setting. Mixed nectarine–peach calibration and plum models performed well in predicting of total soluble solids (TSS) in nectarines and peaches, and plums, respectively. The calibration set samples were scanned at different temperatures (5 and 20 °C) over several seasons to confirm the robustness of these mixed models. Hahn (2004) explored NIR spectral bandwidth effect on Rhizopus stolonifer spores detector and its on-line behavior during classification of red tomatoes. The NIR spectra were acquired before and after inoculating tomatoes in the laboratory. Discriminant analysis carried out at 5, 2, and 1 nm wide spectral bandwidths showed 1 nm bandwidth to possess the highest accuracy (88.92%). When the same was used for on-line classification on an automatic conveyor, a 92% detection accuracy was encountered for a spore count of 6.5 Â 104 sporangiospores mlÀ1. Xie et al. (2007b) used Vis/NIR diffuse reflectance spectroscopy combined with multivariate analysis to differentiate 70 transgenic tomatoes and 94 of their parents. PCA, discriminant analysis (DA), and PLSDA were applied to classify these tomatoes with different genes into two groups. After comparison, PLSDA model with the leaveone-out cross-validation technique after second derivative pre-treatment gave the most satisfactory calibration and prediction ability. Thereafter, Vis/NIR diffuse transmittance spectroscopy, in combination with different chemometrics was used to distinguish transgenic and non-transgenic tomatoes (Xie et al., 2007a). PCA, SIMCA,

discriminant partial least squares (DPLS) regression based on PCA scores were applied to classify these transgenic and non-transgenic tomatoes. When using DPLS after pretreatment of second derivative method, the accuracy could reach 100%, showing Vis/NIR technique to be an effective method to differentiate objects with similar properties. 2.3. Grain and grain products Grains including wheat, rice, and corn are main agricultural products in most countries. Grain quality is an important parameter not only for harvesting, but also for shipping (Burns and Ciurczak, 2001). In many countries, the price of grain is determined by its protein content, starch content, and/or hardness, often with substantial price increments between grades. Several studies show grain quality parameters to be significantly variable, even when harvested in the same field and at the same time (Reyns et al., 2000; Bramble et al., 2002). NIRS technology has made it possible to directly measure different constituentsin the grain products (Wehling et al., 1996; Delwiche, 1998; Campbell et al., 1999; Kawamura et al., 1999; Ber¨ ardo et al., 2005; Ozdemir, 2006). Furthermore, its ability to be installed on the harvesting machine itself is advantageous for on-line determination and grading. Engel et al. (1997) described an approach for inspecting grain protein on-line by the use of NIR analysis. On-line measurement of grain quality with respect to moisture and protein content by a NIR measurement device (Maertens et al., 2004) that was installed in a bypass unit of the clean grain elevator in a conventional combine harvester has been possible (Fig. 3). The calibration models between NIR spectra and quality parameters were developed by PLS algorithm and validated through cross-validation, with standard error of cross-validation (SECV) of 0.57% and 0.31% for protein and moisture content, respectively. Thereafter, with similar equipment, Montes et al. (2006) examined the potential of NIR on combine harvest for determination of dry matter, crude protein, and starch content in maize grain. NIR spectra were collected over a range of 960–1690 nm with the interval of 6 nm, The instrumentation was calibrated by using modified partial least squares (MPLS). In addition, calibration models for determination of dry mater, starch content, in vitro digestibility by cellulase, and soluble sugars in maize forage based on NIR measurements taken directly on the chopper during harvest were developed (Welle et al., 2003). Using a network of six diode arrays, NIR spectrometers were implemented successfully for on-line analysis of dry matter corn grain (Welle et al., 2005). With this method, calibration models were derived from the database of spectra from all six instruments; this eliminated the need to apply specific standardization algorithms when using different NIR instruments. In Japan, Kawamura et al. (2003a) developed another type of automatic rice-quality inspection system using a NIR instrument and a visible light segregator. In the

Fig. 3. Measurement configuration on the bypass of the elevator (Maertens et al., 2004).

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system, the NIR transmission was used to determine moisture and protein content of the samples while the Vis segregator was used to determine sound whole kernel of brown rice. This system enabled rough rice transported to a rice-drying facility to be classified into six qualitative grades. De Temmerman et al. (2007) applied NIR spectroscopy for in-line determination of moisture concentrations in semolina pasta immediately after the extrusion process. Reflectance spectra between 308 and 1704 nm were acquired at the extruded die. PLS regression method was used to develop an adequate prediction model for the inline moisture content. The best cross-validation results were obtained for non-transformed data. The results indicated that NIR spectroscopy could be used for process control in the pasta industry. Besides qualitative and quantitative chemical analysis, NIR spectroscopy technique could also be used for food structure determination. Bruun et al. (2007) applied NIR spectroscopy for monitoring changes in gluten protein structures and interactions when the gluten power is modified by increasing water content and heat treatment. Second-derivative transformation and extended multiplicative spectral signal correction were used as pretreatments of spectra, in order to improving the band resolution and removing physical and quantitative spectral variations. Then PCA and PLS regression method were applied for making classification and calibration models. The results showed NIR spectrum to be able to give important information on structure changes in gluten proteins, including secondary changes. Thereafter, with the similar method mentioned above, the same authors applied NIR spectroscopy for analysis of protein structures and interactions in hydrated gluten, and obtained satisfactory results. Kays et al. (1996) used NIR spectroscopy for the prediction of total dietary fiber in food. Cereal and grain products, including breakfast cereals, flours, bran, crackers, and samples containing commercial oat and wheat fibers, were selected for analysis. These samples were dry milled, and scanned with a NIR spectrometer in the bandwidth range 1100–2800 nm. PLS regression method was applied to develop the models. The results showed that NIR satisfactorily predicted the total dietary fiber content in a wide range of cereal products. 2.4. Dairy products Traditional reference analytical procedures for moisture, fat, protein, and lactose in dairy products are time consuming, expensive, need trained manpower, and fail to comply with requests in modern industry. In order to solve this problem, a lot of instrumental analytical techniques have been developed. From 1980s, middle-infrared spectroscopy technique permitting detection without any previous treatments, and in the absence of chemical regents has indeed revolutionized the dairy laboratories (Kennedy et al., 1985; Luinge et al., 1993). However, this technique is

not suitable for milk powder and other dairy products (Rodriguez-Otero et al., 1997). With developments in computer programming and chemometrics, NIR analysis has been widely used in this area. Furthermore, when coupled with fiber-optics, it can be successfully used for on-line control in the production line. Kawamura et al. (2003b) constructed a NIR spectroscopic sensing system for on-line predicting of three major milk constituents (fat, protein, and lactose), somatic cell count, and milk urea nitrogen in fluid milk. This system consisted of an NIR instrument, a milk flow meter and a milk sampler (Fig. 4), taking the diffusion transmittance spectra in the range of 600–1050 nm at 1 nm intervals every 10 s during milking. This system can be used for real-time monitoring of quality parameters during milking with sufficient precision and accuracy. With the same equipments, a further study (Kawasaki et al., 2005) to improve the robustness of calibration models for on-line measurement of milk quality items using NIR spectrum data were conducted from two dairy herds. It was found that when calibration models developed from data acquired from one herd were used for validation of data from the same herd, the milk quality items could be measured with high levels of accuracy. However, when the calibration models were used for validation of data obtained from the other herd, the accuracy in measurements of all milk analytes except fat was low. Thus, it is very important to use a combined variable sample to develop a robust calibration model. A NIR microspectrometer system for on-line monitoring of fat during milk processing has also been developed (Brennan et al., 2003). This system used Microsystems optical components fabricated using the LIGA technique. These spectrometers have been widely used for color and quality analysis in diamonds, but seldom used for on-line processing detection. NIR spectra were obtained in the range of 800–1100 nm. Evaluation of a number of regression models showed Ridge regression techniques to give best results. Specially designed fiber-optics for on-line NIR measure-

Fig. 4. An on-line NIR spectroscopic sensing system (Kawamura et al., 2003).

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ment of 222 rumen fluid in milking cows (Turza et al., 2002) has been developed. This system could improve the quality of milk, since components in cow’s rumen can be considered as precursors for milk production in milking cows. NIR analysis has also been used in cheese making. Adamopoulos et al. (2001) applied NIR spectroscopic technique for process control of traditional feta cheese during production. NIR spectra were obtained at wavelengths of 1940, 2180, and 2310 nm relating to moisture, protein, and fat, respectively. The calibration models were developed by a suitable computer program and validated using an independent set of analyzed samples. Thereafter, Mertens et al. (2002) proposed a statistical model based on NIR for real-time prediction of cutting time in cheese manufacture, since the cutting point is very important for the process of curd forms (Laporte et al., 1998). In addition, NIR spectrometry combined with electronic nose (EN) data have been used for on-line monitoring of yogurt and filmjolk (a Swedish yogurt-like sour milk) ¨ ´ fermentations under industrial conditions (Navratil et al., 2004). 2.5. Oils Oils are very important food groups. Conventional analytical methods for measuring the oxidation and adulteration of oil are time consuming, destructive, expensive, require chemical reagents, and are laborious. NIR spectroscopy technique has many applications in this area. Yildiz et al. (2001) applied NIR spectroscopy for monitoring oxidation levels in soybean oils. Peroxide value (PV), conjugated diene value (CD), and anisidine value (AV) in soybean oils were quantitatively determined. For the determination, PLS regression and forward stepwise multiple linear regression (FSMLR) combined with first derivative and second derivative methods were used to develop models. They concluded that wavelengths in the 1100–2200 nm regions were most useful for prediction, and PLS regression using first derivative spectra gave the best results for PV. However, as opposed to PV and CD, measurement of AV by NIR was not as well as expected. Thereafter, they (Yildiz et al., 2002) determined PV in corn and soybean oils by NIR spectroscopy technique. When the calibration models developed by PLS regression of first derivative spectra were used to predict validation sets containing equal numbers of corn and soybean oil samples, good results were obtained. Later, NIR spectroscopy was used for measuring degradation products in frying oils, including total polar materials (TPMs), and free fatty acid (FFAs), which have a negative effect on the flavor and nutritional value of fried products (Ng et al., 2007). PLS and FSMLR were used to develop models. The authors found that when using a wavelength at 700–1100 nm, PLS models gave better results than FSMLR models. Moreover, the derivative treatments had limited utility, especially in the longer wavelength regions (1100–

2500 nm). This method could be adapted to an automated, continuous-flow sampling system. Visible and NIR spectroscopy was used for detecting and quantifying sunflower oil adulteration in extra virgin oils (Downey et al., 2002). One-hundred and thirty-eight oil samples were analyzed by Vis/NIR transflectance spectroscopy. A number of mathematical methods were investigated to detect and qualify the sunflower oil adulteration, including hierarchical cluster analysis, SIMCA, and PLS. The accuracy of these mathematical models was compared. SIMCA could successfully discriminate between authentic extra virgin olive and the same oils adulterated with sunflower oil at levels as low as 1% (w/w). Once adulteration was detected, PLS was used to quantitatively analyze the sunflower contents. The results showed that this level of accuracy was acceptable for industrial use. ´ Vis/NIR transmittance spectroscopy was used by Marquez (2003) to determine the total levels of chlorophyll and carotenoid in virgin oil. An initial smoothing technique combined with first derivative treatment was used to correct the signal. PLS regression was used to develop calibration models, which were used to monitor on-line levels of these compounds during virgin olive oil processing in olive oil mills. Satisfactory results were obtained. Thereafter, Marquez et al. (2005) applied NIR transmittance spectroscopy for on-line detection of acid value, bitter taste (k225), and fatty acid compositions in virgin olive oils. NIR spectra were obtained in the wavelength range of 750–2500 nm. A 1 mm optical path length flow cell with a sample volume of 120 ll was used. PLS regression was used to develop models for on-line prediction of all these characteristics. 2.6. Fish and fish products Uddin et al. (2002) applied NIR spectroscopy to assess the end-point temperature (EPT) of heated fish and shellfish meats. In this research, blue marlin, skipjack, red sea bream, kuruma prawn and scallop meats were heat-treated at different temperatures. NIR spectra were measured at the wavelength range of 1100–2500 nm at 2 nm intervals. For calibration, stepwise multiple linear regression was used to develop models. The inference of the water content in the fish meats on the performance was eliminated by selecting appropriate wavelength. A promising linear relationship between the EPT and NIR-predicted temperatures was obtained, revealing the ability of NIR spectroscopy to monitor EPT during the fish and shellfish heating. Thereafter, NIR spectroscopy was used to verify EPT of kamaboko gel (Uddin et al., 2005). PLS and MLR were used to develop model which was tested with validation set. The result showed that NIR-predicted EPT and actual heating temperatures revealed a linear relationship. The models developed by PLS and MLR had similar performance for predicting EPT of kamaboko gel when using appropriate wavelength range. A muli-spectral imaging NIR transflectance system was developed for on-line determination of moisture content in

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dried salted coafish (bacalao) (Wold et al., 2006). The combination of NIR transflectance measurement with spectral imaging allows rather deep penetrating optical sampling and large flexibility in spatial sampling patterns and calibration approaches. In addition, the technique of reflectance, contact transflectance and non-contact trandflectance were compared with a small set of dried salted cod samples. The result showed the last two were superior to reflectance measurements. 2.7. Beverages NIR technique has been used for on-line determination of constituents in alcoholic beverages such as beer, wine, and distilled spirits; nonalcoholic beverages such as fruit juices, teas, and soft drinks; and other products such as infant and adult nutritional formulas. Some of the applications are described below. Recently, Zeaiter et al. (2006) applied Vis/NIR spectroscopy to the study of on-line monitoring the alcohol content during alcoholic wine fermentation. For the determination, samples were scanned in transmission mode over the range of 200–2500 nm at 2 nm intervals using a NIR spectrometer. For calibration, PLS regression method was used to develop the models. In order to correct prediction model used in spectroscopy-based process monitoring, a new method called dynamic orthogonal projection (DOP) was applied. The results showed this method to improve the robustness of the calibration model. NIR spectroscopy combined with multivariate analysis (PCA, DPLS, and linear discriminant analysis (LDA)) has been used for in-line monitoring the progress of red wine fermentation in a pilot scale (Cozzolino et al., 2006). Samples (n = 652) were collected at different times from several pilot scale fermentations, and scanned in transmission mode with the spectra range between 400 and 2500 nm. They used PCA to demonstrate consistent progressive spectral changes that occur through the time course of the fermentation. Linear LDA showed that regardless of variety or vintage, samples belonging to a particular time point in fermentation could be correctly classified. In addition, continuous processing of apple, grape, pear, apple–cherry and apple–banana juices for soluble solids and total solids/total moisture can also be assessed (Singh et al., 1996). Three in-line sensors: NIR, guided microwave and Maselli refractometer were compared for their in-line performance of testing. The result showed NIR and guided microwave to be good for assessing the soluble and total solids, and Maselli refractometer to be excellent for predicting soluble solids under different operating conditions. ´ Leon et al. (2005) applied NIR transflectance spectroscopy for detection of adulteration of apple juice samples. Two types of adulterants were assessed: a high fructose corn syrup (HFCS) and a sugar solution. DPLS regression method was used. The results showed that the accuracy of detection of authentic apple juice and adulterated apple juice were 86–100% and 91–100%, respectively, depending on the adulterant type and level of adulteration.

2.8. Others On-line application using NIR methods on other kinds of food are also known. Although these foods are not among the five categories mentioned above, the methodology and interpretation there from are very important and should not be ignored. NIR methods have been used for on-line viscosity and conductivity measurements in frozen model sorbet in a continuous freezer/extrusion process (Bolliger et al., 1998). Monitoring of colour and composition in an extruder during the extrusion of yellow corn flour (Apruzzese et al., 2000), and on-line classification of poultry carcass quality (Chen et al., 2003) by Vis/NIR spectrophotometer system has been known. In baking area, Sinelli et al. (2004) used FT-NIR spectrometer with an optic probe for monitoring the kinetics of dough proofing and bread staling. 2.9. Constraints of NIR techniques in food analysis Although the operating cost of NIRS is low, the instrument itself is highly priced; this limits its practical application. Efforts by researchers and industrial organizations to develop simple and low-cost instruments could revolutionize the use of NIR techniques for on/in-line quality monitoring of foods. Some calibration models based on NIR spectroscopy, especially for on-line application, are not reliable and stable enough when used practically. Hence, it is imperative for researchers to choose proper chemometrics to build robust models. In some cases, conventional methods may not offer a satisfactory solution to a given problem due to complexity of the data. This also necessitates the development of new chemometric methods so as to further improve the reliability and accuracy of the calibration models. In addition, there are other limitations of NIR spectroscopy technique. The technique is not sensitive to the mineral content, since there is no absorbtion of minerals in the NIR spectrum region. An alternative way to solve this problem efficiently is to combine different detection techniques with NIR spectroscopy, such as X-ray fluorescence spectroscopy, UV light, and electronic nose technique. Some papers describing the use of a combination of techniques using different detection methods have been ´ published in recent years (Cimander et al., 2002; Navratil et al., 2004), although more efforts should be made to solve this issue. 2.10. Conclusions and future outlook On/in line applications of NIR spectroscopy in food science are reviewed in meats, fruit and vegetables, grain, and grain products, milk and dairy products, and beverages and other areas. At present, NIR technique is widely accepted as one of the most promising on/in-line process control techniques NIR is obviously a nondestructive,

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reliable and accurate technique for monitoring chemical and physical parameters during food processing. Furthermore, it is worth mentioning that the appearance of fiberoptic probes significantly improves the ability of NIR techniques to monitor and control processes especially using remote on/in line detection. Acknowledgements The authors gratefully acknowledge the financial support provided by National Natural Science Foundation of China (No. 30671197) and National Key Technology R&D Program (No. 2006BAD11A12). References
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