Chapter 14

Quality Parameters and Quality Control Methodologies

For any food product, quality is subjected to consumer perceptions of taste, mouthfeel and colour. This is also true for coconut liquid products. As coconut water, milk and cream are increasingly consumed worldwide, the quality of coconut liquid products can be better determined by objective assessments. 

Several quality parameters, which differ in chemical composition, can define the makeup of each product. These parameters refer to the chemical, microbiological, nutritional and physical factors that make up the coconut liquid products its unique properties, which also influences the products shelf life. For example, as coconut water and milk are low-acid and high water activity foods, they become highly susceptible to microbial spoilage and deterioration. 

That said, research studies are still not extensive enough to cover all aspects of coconut liquid products. Therefore, this chapter serves as a guide by attempting to consolidate and recommend possible quality control methods to objectively define coconut liquid products and suggest a range of values for each parameter. It is important that experienced quality control personnel and statisticians are employed to conduct quality checks and shelf life studies for these products. 

The recommended quality control parameters are shown in Table 14.1. All tests should be done before and after aseptic processing and packaging. However, for boxes which are not ticked, it is optional or of less importance to do so for the respective products. Analytical methods for the respective quality parameters are also recommended in CODEX STAN 247-2005, unless otherwise stated. 

Table 14.1

Important quality control tests for liquid coconut products

Table 14.1 Important quality control tests for liquid coconut products
TEST COCONUT WATER BASED PRODUCTS COCONUT MILK BASED PRODUCTS
Flavour/odour
Total soluble solids °Brix
Dry matter determination
pH/ titratable acidity
Microbiological content
Sulphite test
Browning index determination
Optical density/ Turbidity test
Free fatty acids determination
Viscosity

Besides flavour, all listed parameters can be determined by standard methods of analysis to give meaningful and reliable results. This is because flavour and odour are commonly evaluated by sensory means, usually by groups of panellists. These analysis methods were collected and published in books such as Guidelines for Sensory Analysis in Food Product Development and Quality Control (Carpenter et al., 2008) and Sensory Evaluation by Quantitative Descriptive Analysis (Stone et al., 1974). 

The suggested range of values are not applicable to all coconut types and varieties. They could be subjected to variations in coconut maturity, variety, cultivation practices and more. In addition, post- harvest factors, such as packaging, transportation and storage conditions can also influence the composition of coconut liquid products. 

Quality control methodologies and suggested quality parameters

Total soluble solids

Total soluble solids is an important quality parameter in many food products. Its analysis is also a commonly practiced one. It typically indicates the amount of dissolved sugars in the product, thus affecting both safety and hedonic properties. It can be measured using a refractometer, which calculates the total soluble solids of the sample in °Brix, and is more important for coconut water. 

Table 14.2

Table 14.1.2 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED °BRIX RANGE
Young coconut water (7-9 months) 5.5-8.0
Mature coconut water (10-13 months) 3.5-6.0

Dry matter or total solids analysis

The analysis for dry matter or total solids can be done by oven or infrared drying. In oven drying, direct heating is used to dry the sample, followed by manual weighing. These analyses are more so important for coconut milk and cream, which standards have been defined by CODEX STAN 240-2003.

Infrared drying is a fast method of dry matter or total solids analysis. It is a faster method compared to oven drying.

Table 14.3

Dry matter analysis methods

Table 14.2 Dry matter analysis methods
TEST METHOD PROCEDURE
Oven drying The sample is weighed before and after drying, and drying takes place in an oven. Knowing the difference in original and dried weight corresponds with the moisture mass, and the percentage of dry matter can be calculated.
Infrared drying An infrared or halogen moisture analyser is an automated machine which gives the moisture or dry content reading of the sample without a need for further manual calculation.

Table 14.4

Table 14.2.2 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED PERCENTAGE RANGE OF TOTAL SOLIDS
Light coconut milk 6.6-12.6
Coconut milk 12.7-25.3
Coconut cream 25.4-37.3

pH measurement

pH is a crucial parameter for food as it indicates the sourness of a product and its current shelf life stability. For coconut water and milk, the pH measurement drops over the course of its shelf life, until it is exceeded. Using a calibrated pH meter, the pH of a sample may be measured.

Table 14.5

Table 14.2.3 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED pH RANGE
Young coconut water (7-9 months) 4.5-5.3
Mature coconut water (10-13 months) 5.3-5.8
Coconut milk and cream At least 5.9

Titratable acidity (TA)

In coconut water, TA is expressed as the percentage of malic acid equivalent. More specifically, TA is determined as the malic acid equivalent by titration of a sample against 0.1N NaOH. The sample is titrated until pH 8.2. The sample can be diluted where required.

Note 14.1

Table 14.6

Table 14.2.4 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED % OF TITRATABLE ACIDITY
Young coconut water (7-9 months) 0.07-0.09
Mature coconut water (10-13 months) 0.05-0.08

Microbiological testing

Microbiological testing can be measured as the Total Aerobic Count (APC), as well as Yeast and Mould Plate Count (YMPC). First, samples are collected and used to prepare serial dilutions of the samples. Then, diluted samples buffered at pH 7.2 are placed onto agar plates or petri films with different kinds of nutrient media available to culture microorganisms for APC and YMPC. 

Thereafter, the diluted samples are incubated at 37°C for
24-48 hours for APC. For YMPC, they are incubated at 25°C for
3-5 days, or as stipulated by regulations (US FDA, 2001). Taking into account the dilution factor, the colony forming units are calculated in the original sample and checked against the local authority’s compliance standards for quality control. 

Sulphite test

Sulphite test can be used to determine the amount of sulphite residue in coconut water, milk and beverages. There are many ways to do so. In this chapter, we will cover two methods, using sulphite test strips and DTNB test. For a faster and approximated result, sulphite test strips may be used. For a more accurate result, the DTNB test may be used.

Table 14.7

Sulphite test methods

Ellman’s reagent - 5,5’-Dithiobis-(2-Nitrobenzoic Acid)

Table 14.3 Sulphite test methods
TEST METHOD PROCEDURE
Sulphite Test Strip First dip the test strip into the sample. Compare the colour of the strip with the standard printed on test package after a stipulated amount of time (e.g. 30 seconds). Depending on the test strip supplier, the instructions might vary slightly.
DTNB Test For the standard curve construction, first prepare the DTNB1 solution, diluted in phosphate buffered saline solution (pH 7.2). Then prepare the standard solutions of 0.1 to 5 ppm sodium metabisulfite. For 1 mL of each of these standard solutions, add 1mL of DTNB and top up to 10 mL with distilled water. From these standard solutions, record the absorbance at 412 nm after 5 minutes of reaction at room temperature. Finally, construct a standard curve of absorbance against SMB concentrations.

For sulphite content measurement, mix 0.5 mL of sample solution with 1mL of DTNB and top it up to 10 mL with distilled water first. Record the absorbance at 412 nm after 5 minutes. Using the standard curve, find the concentration of the diluted sample.

Note that the volume of coconut sample used for the reaction may be adjusted as necessary for the absorbance result to fall within the range of the standard curve.

DTNB Test

The residual levels of sulphite in the coconut liquid products are regulated by laws and changes between countries. It is recommended to consult with the regulatory experts in the respective countries.

Colour

Browning in coconut water 
Browning is an especially prevalent problem in coconut water. It is a visual component of the product that is often used as an indicator of shelf life acceptability, even though browning by itself may not be indicative of product spoilage. The browning index reflects the cumulative browning of all pathways, including enzymatic and non- enzymatic occurrences in coconut water. Examples are Maillard reaction and ascorbic acid browning. The standard for acceptable browning is set by the individual company or customers. 

The browning index (BI) is calculated as the difference between the absorbance at 420 nm and 550 nm (to correct for turbidity). The absorbance of the samples is first recorded at 420nm (A420) and 550nm (A550), then the Browning index is calculated. 

Image 14.1

Note 14.2

Using samples with different degrees of browning, construct a browning scale index and establish a standard. For example, Index 9 of BI 0.055 (Figure 14.1).

Figure 14.1

Browning index scale for coconut water

Pinking in coconut water 
Pinking is caused by an intermediate in the polyphenol oxidase- catalysed browning reaction and is typically found in young coconut water only. It is an indication of cracks in young coconut, which lead to the exposure of coconut water to the external environment. 

Table 14.8

Table 14.3.2 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED COLOUR STANDARD
Young coconut water (7-9 months) Should not be pink, if browning occurs less than index 9 of BI 0.055
Mature coconut water (10-13 months) Less than index 9 of BI 0.055

Discolouration in coconut milk 
Coconut milk normally appears as creamy white. Due to reactions such as browning, it may be discoloured, forming a brown, greyish or off-white colour. The colour of coconut milk is also affected by oil globules. In general, when there are small and numerous droplets, the reflectance off the oil globules gives a white colour. 

The colour of coconut milk can be analysed by measuring the reflectance with a colorimeter to obtain three Hunter parameters, namely “L” lightness, “a” red or green component and “b” yellow or blue component. L and b can be used to describe the change in colour of coconut milk (Chiewchan, 2005). A two-axis scale can also be set up for the colour of coconut milk using “L” and “b” values. Although tedious, this scale is valuable to have. 

Studies show that for coconut milk, the “L” values can range from 70.5-88.0 while “b” values can range from 4.2-8.6. The values are affected by homogenization and different temperatures. For example, homogenization has shown an increase in lightness at 30°C when “L” values in coconut milk increased from 77.92 up to 80.59. (Chiewchan, 2005; Waisundara et al., 2006)

Optical density or turbidity test 

Optical density can be used as a measure to indicate the colour of the product sample. A cut-off point above or below a sample is deemed to have passed its shelf life. It should be determined by the specific product requirements. Using an appropriately calibrated spectrophotometer, absorbance of samples are recorded at 600 nm. Using a series of samples from various times in its shelf life, set a standard for quality control of the sample. 

Turbidity is an important quality parameter for coconut water, as customer’s acceptability may decrease as turbidity increases. Turbidity can be measured using a turbidimeter to establish a standard. This is a faster method to measure the clarity levels of coconut liquid products. This test is more important for coconut water as coconut milk is naturally opaque. 

Table 14.9

Table 14.3.3 (inget namn)
COCONUT LIQUID PRODUCT SUGGESTED TURBIDITY (NTU)
Young coconut water (7 - 9 months) Less than 50
Mature coconut water (10 - 13 months) Less than 100

Free fatty acids (FFA) measurement 

FFA is commonly a product of fat hydrolysis. It is therefore an indicator of spoilage in foods. The presence of FFA is usually associated with the onset of rancidity and off-flavour development, which is especially important in foods with significant fat content, such as coconut milk and cream. 

Titration method is used to measure FFA content in a food sample. First, titration of the product is carried out against a standard NaOH solution, with phenolphtalein as an indicator. For coconut products, FFA is usually a reflection of its free lauric acid content which has a major presence. 

More commonly, free fatty acid (FFA) values are specified for desiccated coconut and coconut cream powder products. They are a maximum of 0.2 and 0.3% respectively. Some specifications for coconut cream show FFA content to be a maximum of 0.15%.

Note 14.3

* Please note that the sample may be diluted as necessary

* Please note that the sample may be diluted as necessary

Viscosity measurement 

Viscosity measurement is used to determine the thickness of the product, thus relating to the filling component in the production run, as well as the product’s mouthfeel and stability. Using a temperature controlled Brookfield viscometer, the viscosity of a product can be measured at different shear rates. These measurements characterize the rheological behaviour of the tested sample and are important in the designing and fine tuning of aseptic line solutions in terms of packaging and processing equipment. This measurement is more applicable for coconut milk and cream, where the product can be very thick, depending on the formulation and process parameters (e.g. homogenization pressure). It is generally observed that coconut milk and cream increase its viscosity with storage time. Please refer to Chapter 10 for more details. 

Note 
Viscosity affects the pourability of the product from the package. There are no suggested ranges for the viscosity of coconut cream. Analysis of commercial samples at Tetra Pak in-house rheology lab (RheoLab) shows that, at a shear rate of 100s-1 with temperature of 30°C between 17-25.1% of oil content, the viscosity of coconut milk can range from as low as 8 mPas to as high as 260 mPas. 

Note 14.4

Accelerated shelf life

Coconut liquid products are packaged to maintain quality during its defined shelf life conditions. Shelf life depends on several factors, such as raw material quality, processing parameters, storage conditions and the threshold of acceptance of the individual consumer. It cannot be determined in terms of time by the packaging material supplier. Although processing and packaging can protect the contents, it cannot improve the quality of the coconut liquid products if they were produced from bad raw materials. 

Accelerated shelf life determination (ASLD)

ASLD is used to shorten the time required to estimate a shelf life, which otherwise can take an unrealistically long time to determine. As the food trade globalizes and competition in the food market intensifies at national and international levels, there is a greater need to quickly determine shelf life within a shorter time period. This situation becomes more pressing when shelf life is expected to range from several months to a few years. Therefore, the set up for ASLD usually involves increasing the product’s storage temperature to accelerate time required to reach the end of its shelf life. 

The typical storage temperature for ASLD studies are as follows: 

Table 14.10

Typical storage temperature for ASLD study

Table 14.4 Typical storage temperature for ASLD study
FOOD CATEGORY CONTROL TEMPERATURE (°C) ASLD TEMPERATURE RANGE (°C)
Refrigerated 2 5-15
Shelf-stable 22 30-45

As most reaction rates increase exponentially with a rise in temperature, increasing the temperature by 10°C can cause quality loss to increase by a factor of 2-6. This simplified factor, known as Q10, depends on the food being evaluated, the mode of failure, and the temperature range. 

To calculate the Q10 factor, the product is stored at three to four different temperatures within the specified range. Each temperature is constantly maintained within 1°C, and the ASLD temperature range is usually raised slightly above the control temperature. This helps to avoid changes in the product failure mode. 

Besides elevated temperatures, additional ASLD conditions are also occasionally employed. These include elevated humidity, oxygen tension in the headspace and cycling temperature fluctuations. However, the complexity of these factors requires special mathematical data manipulation, which makes their application quite cumbersome. 

Accelerated shelf life testing requires careful methodology. As such, a number of test conditions must first be made before the study. 

TEST CONDITIONS OF ACCELERATED SHELF LIFE TESTING

*Source: Graf et al.,1991

1. The appropriate quality factor or index of deterioration

a. For example, the maximum microbial count limit set by the 
authority, or maximum browning index as the maximum acceptable limit

2. Storage temperature

3. Additional ASLD conditions a. For example, humidity

4. Control and the number of replicates

5. Total storage time

6. Number of variables
a. For example, coconut water with or without antioxidants

7. Kinetic models


Recommended experimental set-up for coconut liquid products

After a specified treatment and storage duration, the recommended experimental set-up for the estimation of shelf life is as follows:

Table 14.11

Recommended temperatures for shelf life study

Table 14.5
STORAGE TEMPERATURE (°C) EQUIPMENT
4 Refrigerated incubator
25 Refrigerated incubator
30 High temperature incubator
40 High temperature incubator
55 High temperature incubator

Table 14.12

Recommended intervals for the shelf life study of coconut liquid products

Table 14.6
WEEK NO. INTERVALS (NO. OF WEEKS) TEMPERATURE (°C) #colspan# #colspan# #colspan# #colspan#
4 25 30 40 55
0 -
1 1
2 1
4 2
6 2
8 2
12 4
16 4
20 4
24 4
28 4

In general, it is expected that products stored at higher temperatures will have a shorter shelf life. Thus, shelf life study for samples stored at higher temperatures may end sooner. In comparison, samples stored at 4°C can be expected to last at least three months without any significant change in quality. Tables 14.11 and 14.12 may be adjusted to fit the conditions where necessary. 

The browning index of coconut water as a limiting factor to determine the shelf life of long life coconut water is illustrated below. First, packed coconut water samples at four different temperatures are stored for up to seven months (28 weeks). At each storage interval, samples are removed and analysed for the browning index. When stored, there will be a gradual increase in the browning index of the coconut water throughout the storage period.

A RELATIONSHIP BETWEEN SHELF LIFE AND BROWNING INDEX CAN BE DETERMINED WITH THE FOLLOWING STEPS:

1. Record absorbance of the samples at 420nm (A420) and 550nm (A550), and calculate the Browning index.

Browning index (BI) = A420 - A550

2. Determine the rate of reaction at each storage temperature by plotting a graph of browning index (ln A/A0) against storage duration.

a) Where A is the browning index of the sample and A0 is initial 
browning index

3. From this graph, the reaction rate is obtained as:
a) Slope = -k, where k is the reaction rate for each storage 
temperature

4. Repeat steps 2 and 3 for a minimum of three storage temperatures. Based on the k values obtained from the different storage temperatures, plot shelf life against storage temperature on
the graph.

Shelf life is calculated based on the following equation:

Note 14.5

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