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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121 SPECTRAL ANALYSIS OF CHILLI POWDER TO DETECT THE PRESENCE OF ADULTERANTS K.Kaleeswari 1 , Dr.S.Vasantharathna 2 1 (Department of ECE, PG Student, Coimbatore Institute of Technology, Coimbatore, India,[email protected]) 2 (Department of ECE, HOD, Coimbatore Institute of Technology, Coimbatore, India, [email protected]) ______________________________________________________________________________________________________ AbstractDetection of adulterants in food products is mandatory to ensure that the food we consume is of good quality. In case the adulterant is not detected properly, it leads to various health hazards and fatal diseases. This project focuses on analysing the presence of adulterants in chilli powder, one of the most commonly used ingredient in our household. The common adulterants used in chilli powder are Red lead salt, Sudan dyes, Brick powder etc,. Conventionally chemical tests were being conducted to detect these chemicals. In the proposed work spectral properties of materials are used to identify the adulterants using NIR Spectroscopy. NIR spectroscopy which is primarily used in material science applications is used here to perform analysis of various food adulterants. In the proposed work presence of adulterants like Red lead salt, and Brick powder were found and the quantity of these adulterants were also measured. By this detection process it is possible to avoid using the food stuffs with more quantity of adulterants. Keywords— NIR spectroscopy, Red lead salt, Brick powder, Spectral Properties, Reflectance, Transmittance, MATLAB. _________________________________________________________________________________________________________________ 1. INTRODUCTION Adulteration in food products is the most serious problem in food quality control. In India there are many agencies to monitor the Food Safety and Food Security like International Association for Food Protection, Food Safety and Security Authority of India, International Food Information Centre, etc. These agencies use different techniques to determine the food quality. One of the main factors affecting the quality of food is the addition of adulterants in food products. Food adulteration is an act of intentionally debasing the quality of food offered for sale either by substitution of inferior substances or removal of some valuable agents. It includes the food that contains any poisonous or deleterious substance or a pesticide chemical residue that is unsafe or unsafe colour additive which may render it injurious to health. Adulteration in chilli powder became much predominant in present days. In order to increase the quantity of chilli powder, various adulterants like brick powder, maida, flour, wheat flour etc., are added. To improve the colour of chilli powder many colouring agents which are able to give red colour to chilli powder are added. Basically the colouring matter in food may be natural or synthetic. They may also be classified as water soluble and oil soluble. Natural colours consist of chlorophyll, Carotenes, Curcumin, Caramel, Annatto, Capsainthin etc. Synthetic colours are of importance as they are widely used in different foods. Synthetic colours are further classified as acidic and basic dyes. Only eight coal-tar food colours are permitted in certain food products under the provision of Food Adulteration Act (1954). They include three Red shades namely, Carmoisine, Ponceau 4R, Erythrosine, two yellow shades Sunset yellow-FCF and Tartrazine, two blue shades Brilliant Blue FCF and Indigo Carmine and one green shade i.e. Fast green FCF. However certain unpermitted colours such as metanil yellow, Rhodamine B, Orange G, Red Lead, Blue VRS, Sudan Dyes and certain oil soluble colors are often added in foods as adulterants. These unpermitted dyes lead to hazardous ill effects. So detection of the adulterants present in chilli powder is most important. There are various techniques available to detect the presence of adulterants in food products. Spectroscopic Techniques such as Fourier transform Infra Red (FTIR) spectroscopy, fluorescence spectroscopy, mid-infrared (MIR) spectroscopy and near-infrared (NIR) spectroscopy are useful for characterization and detection of adulterants. Thin layer chromatography is used to detect the presence of Sudan dyes in chilli powder [3]. The NIR spectroscopy and Raman spectroscopy was used to detect the Sudan dyes present in chilli powder [2]. The NIR spectroscopy was used to detect the jaggery syrup in honey [1]. The NMR Spectroscopy was used to detect adulteration in milk [5]. Electronic nose and Tongue are used to identify the adulterants present in different food products. 2. SAMPLE PREPARATION Three different brands of chilli powder were purchased from the local market and one sample was prepared by grinding the whole chilli purchased from the market. Various samples were prepared by adding the adulterant at various proportion with the chilli powder. Totally 56 samples were prepared by adding two adulterant ie, Red lead and brick powder at different proportion. The table given below represents the sample details. Table1: Proportion of chilli powder and adulterant % of Adulteration Amount of chilli powder in grams Amount of adulterant added in grams 0 3 0 10 2.7 0.3 20 2.4 0.6 30 2.1 0.9 40 1.8 1.2 50 1.5 1.5 Volume: 03 Issue: 06 2016 www.ijmtes.com 145

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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121

SPECTRAL ANALYSIS OF CHILLI POWDER TO DETECT THE PRESENCE OF ADULTERANTS

K.Kaleeswari1, Dr.S.Vasantharathna2 1(Department of ECE, PG Student, Coimbatore Institute of Technology, Coimbatore,

India,[email protected]) 2(Department of ECE, HOD, Coimbatore Institute of Technology, Coimbatore, India, [email protected])

______________________________________________________________________________________________________

Abstract—Detection of adulterants in food products is mandatory to ensure that the food we consume is of good quality. In case the adulterant is not detected properly, it leads to various health hazards and fatal diseases. This project focuses on analysing the presence of adulterants in chilli powder, one of the most commonly used ingredient in our household. The common adulterants used in chilli powder are Red lead salt, Sudan dyes, Brick powder etc,. Conventionally chemical tests were being conducted to detect these chemicals. In the proposed work spectral properties of materials are used to identify the adulterants using NIR Spectroscopy. NIR spectroscopy which is primarily used in material science applications is used here to perform analysis of various food adulterants. In the proposed work presence of adulterants like Red lead salt, and Brick powder were found and the quantity of these adulterants were also measured. By this detection process it is possible to avoid using the food stuffs with more quantity of adulterants.

Keywords— NIR spectroscopy, Red lead salt, Brick powder, Spectral Properties, Reflectance, Transmittance, MATLAB. _________________________________________________________________________________________________________________

1. INTRODUCTION Adulteration in food products is the most serious problem in food quality control. In India there are many agencies to monitor the Food Safety and Food Security like International Association for Food Protection, Food Safety and Security Authority of India, International Food Information Centre, etc. These agencies use different techniques to determine the food quality. One of the main factors affecting the quality of food is the addition of adulterants in food products. Food adulteration is an act of intentionally debasing the quality of food offered for sale either by substitution of inferior substances or removal of some valuable agents. It includes the food that contains any poisonous or deleterious substance or a pesticide chemical residue that is unsafe or unsafe colour additive which may render it injurious to health. Adulteration in chilli powder became much predominant in present days. In order to increase the quantity of chilli powder, various adulterants like brick powder, maida, flour, wheat flour etc., are added. To improve the colour of chilli powder many colouring agents which are able to give red colour to chilli powder are added. Basically the colouring matter in food may be natural or synthetic. They may also be classified as water soluble and oil soluble. Natural colours consist of chlorophyll, Carotenes, Curcumin, Caramel, Annatto, Capsainthin etc. Synthetic colours are of importance as they are widely used in different foods. Synthetic colours are further classified as acidic and basic dyes. Only eight coal-tar food colours are permitted in certain food products under the provision of Food Adulteration Act (1954). They include three Red shades namely, Carmoisine, Ponceau 4R, Erythrosine, two yellow shades Sunset yellow-FCF and Tartrazine, two blue shades Brilliant Blue FCF and Indigo Carmine and one green shade i.e. Fast green FCF. However certain unpermitted colours such as metanil yellow, Rhodamine B, Orange G, Red Lead, Blue VRS, Sudan Dyes and certain oil soluble colors are often added in foods as adulterants.

These unpermitted dyes lead to hazardous ill effects. So detection of the adulterants present in chilli powder is most important. There are various techniques available to detect the presence of adulterants in food products. Spectroscopic Techniques such as Fourier transform Infra Red (FTIR) spectroscopy, fluorescence spectroscopy, mid-infrared (MIR) spectroscopy and near-infrared (NIR) spectroscopy are useful for characterization and detection of adulterants. Thin layer chromatography is used to detect the presence of Sudan dyes in chilli powder [3]. The NIR spectroscopy and Raman spectroscopy was used to detect the Sudan dyes present in chilli powder [2]. The NIR spectroscopy was used to detect the jaggery syrup in honey [1]. The NMR Spectroscopy was used to detect adulteration in milk [5]. Electronic nose and Tongue are used to identify the adulterants present in different food products.

2. SAMPLE PREPARATION Three different brands of chilli powder were purchased from the local market and one sample was prepared by grinding the whole chilli purchased from the market. Various samples were prepared by adding the adulterant at various proportion with the chilli powder. Totally 56 samples were prepared by adding two adulterant ie, Red lead and brick powder at different proportion. The table given below represents the sample details. Table1: Proportion of chilli powder and adulterant % of Adulteration Amount of chilli

powder in grams

Amount of adulterant added

in grams 0 3 0 10 2.7 0.3 20 2.4 0.6 30 2.1 0.9 40 1.8 1.2 50 1.5 1.5

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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121

3. CHEMICAL TEST AND RESULTS Chemical test was done to determine the possibility of presence of adulterants. [1] Detection of Red Lead in chilli powder To a sample of chilli powder, add dil. HNO3. Filter the solution and add 2 drops of potassium iodide solution to the filtrate. Yellow ppt. indicates the presence of lead salts in chilli powder. [2] Detection of Brick powder in chilli powder Method I: Add small amount of given red chilli powder in beaker containing water. Brick powder settles at the bottom while pure chilli powder floats over water. Method II: To a little powder of chilli add small amount of concentrated HCl and mix to the consistency of paste, dip the rear end of the match stick into the paste and hold over the flame, brick red color flame indicates the presence of brick powder. The below table represents the chemical test results for various samples taken. Table 2: Chemical test result for various brands of chilli powder

Brand Name Result For Red Lead Test

Results For Brick Powder Test

Home Made Yellow Precipitate Was Not Formed

No Brick Color Flame Produced

Brand 1 Yellow Precipitate Was Not Formed

No Brick Color Flame Produced

Brand 2 Yellow Dots Were Found

No Brick Color Flame Produced

Brand 3 Yellow Precipitate Was Formed

No Brick Color Flame Produced

This table shows that the home made chilli powder and Brand 1 chilli powder does not have red lead as adulterant and Brand2 has small amount of adulterant as compared to the home made chilli powder and Brand2 is highly adulterated with Red lead.

4. NIR INSTRUMENTATION Near Infrared Spectroscopy is used in many industries including the pharmaceutical, petrochemical, agriculture, cosmetics, chemical and food industries. However in the food industry NIR has an almost universal application. Since food is made mostly from proteins, carbohydrates, fats and water, i.e. >99% by weight, NIR provides a means of measuring these components in almost any food. THREE NIR REGIONS Figure 1. Shows the NIR region from 720 to 2500nm. There are three parts of the NIR spectral region, 1) Reflectance, 2) Transmission and 3) Transflectance. TRANSFLECTANCE: 720 to 1100nm. This section is most suited to transflectance through a thick sample, such as, seeds, slurries, liquids and pastes. The absorption bands are due to 3rd overtones of the fundamental stretch bonds in the Mid IR region. TRANSMISSION: 1200 to 1850nm. This section can be used for transmission through liquids and films, as well as diffuse reflectance measurements off samples with high

water contents. The absorption bands are due to the 1st and 2nd overtones of the fundamental stretch bonds in the Mid IR region REFLECTANCE: 1850 to 2500nm. This section is predominantly used for making diffuse reflectance measurements off ground or solid materials. The absorption bands are due to combination bands, i.e., C-H stretch and bend combination bands. Figure 2. Shows part of the electromagnetic radiation spectrum from 300nm to 10000nm. It shows the Visible, NIR and Mid IR spectral regions. \

Fig 1: NIR regions

Fig 2: Electromagnetic Spectrum

5. HARDWARE SPECIFICATION Jasco V-570 UV/VIS/NIR spectroscopy was used to test the sample. The specifications of Jasco V-570 is listed in table 3.

Table 3: Hardware specification

Visible Near Infrared Mid Infrared

Electronic

Overtone and Fundamental

Combination Bands

Vibrational

Shift

Bands 400 750

1000 1750 2000 2500 10000

Wavelength (Nanometers)

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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121

The samples were tested in the Jasco Spectrometer by taking a small amount of sample between the two glass plates at source side of spectroscopy. Two empty glass plates were tied together and kept at a reference. The light of different wavelength was passing through the sample and the absorbance was calcuted for all wavelengths. Formula for calculating absorbance at a particular wavelength was given as, Absorbance= log (Intensity of Light incident on the sample/ Intensity of light transmitted from the sample) The hardware setup for testing the sample was shown in figure 3.

Fig 3: Hardware setup

Fig 4: Spectrum of sample

6. RESULTS Totally 56 samples were tested and analyzed using MATLAB -2010a software. The wavelength Vs Absorbance curve for various samples was shown as below. Figure 5 represents the graph showing homemade chilli powder adulterated with 10%,20%,30%,40%,50% of red lead.

Fig 5:Home made chilli powder adulterated with red lead Figure 6 represents the graph showing homemade chilli powder adulterated with 10%,20%,30%,40%,50% of Brick powder.

Fig 6:Home made chilli powder adulterated with Brick powder Figure 7 represents the graph showing home made chilli powder adulterated with 10%,20%,30%,40%,50% of red lead and brick powder.

Fig 7:Home made chilli powder adulterated with red lead and brick powder

Parameter Specification Optical System Double beam system with

single monochromatic (190 to 2500nm)

Light Source Halogen lamp (330 to 2500nm)

Scanning Speed 32000 nm/min Power requirement 100, 115, 200, 220, 230 and

240 V Dimension and weight Pbs unit: 100(W) x 170(D) x

125(H) mm, 1.9 Kg

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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121

In the same manner the samples of Brand1, Brand2, and Brand3 chilli powders were tested and analyzed. The Absorbance value for each sample varies with respect to the percentage of adulterant present in that sample. For Chilli powders only there is a negative peak at wavelength range of 306 to 309nm. For example figure 8 shows the graph for turmeric powder. There was no negative peak at particular wavelengths for turmeric powder. For different proportion of red lead added, the negative peak value was changed. Similarly for brick powder there was a positive peak at wavelength range of 685 to 695 nm. The absorbance values for various samples were listed in Table 4 ,5 and 6. Brand Name Percentage of

adulteration Wavelength in

nm Absorbance

Home made 0 306 -0.5448 10 307 -0.5311 20 307 -0.5186 30 306 -0.4793 40 307 -0.4553 50 307 -0.1850

Table 4: Absorbance and wavelength values at which negative peak occurs when adding red lead as an adulterant Brand Name Percentage of

adulteration Wavelength in

nm Absorbance

Home made 0 683 -0.0111 10 685 0.1376 20 686 0.1888 30 688 0.219 40 687 0.3135 50 686 0.3835

Table 5: Absorbance and wavelength values at which positive peak occurs when adding brick powder as an adulterant Table 6: Absorbance and wavelength values at which positive peak occurs when adding brick powder as an adulterant and negative peak occurs when red lead as an adulterants Similarly for three brands of chilli powder the peak values and wavelengths were taken. For red lead the negative peak goes upward as adulteration increases and for brick powder the positive peak goes upward as adulteration increased. Considering the home made powder as reference the three brands of chilli powder were analyzed for detecting the adulterants. Based on this a model was developed for identifying the adulterants present in chilli powder. Figures 8,9,10 represents the software model developed for identifying red lead and brick powder.

Fig 8: Selection of wavelength and obtained absorbance stored in a excel sheet

Fig 9: Output obtained when Turmeric powder data as input

Fig 10: Output obtained when chilli powder adulterated with brick powder given as input Conclusion Thus the NIR spectroscopy was effectively used to detect the presence of adulterants in chilli powder and it is a non invasive method for detecting the adulterants. The main advantages of this method is time taken to analyse the sample is very less and the amount of sample taken for test is also very less. In the proposed work results are carried out using MATLAB software. In future, a hardware can be developed to detect the adulterants and the expiry of the

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IJMTES | International Journal of Modern Trends in Engineering and Science ISSN: 2348-3121

chilli powder can also be determined by using this NIR spectroscopy method.

REFERENCES

[1] Sunita Mishra, Uma Kamboj, Harpreet Kaur and Pawan Kapur, “Detection of jaggery syrup in honey using near-infrared spectroscopy ” , International Journal of Food Sciences and Nutrition, May 2010; 61(3): 306–315 .

[2] Pamela Galvin-King , Yen-Cheng Ho , Steven E.J. Bell , Christopher T. Elliott and Simon A. Haughey, “The feasibility of using near infrared and Raman spectroscopic techniques to detect fraudulent adulteration of chili powders with Sudan dye”, Science Direct.com, doi:10.1016/j.foodcont.2014.03.047.

[3] M Masarat Dar, Wani Idrees and FA Masoodi Dar, “Detection of Sudan Dyes in Red Chilli Powder by Thin Layer Chromatography”, Open Access Scientific Reports, http://dx.doi.org/10.4172/scientificreports.586.

[4] R. Fugel, R. Carle and A. Schieber, “Quality and authenticity control of fruit purees, fruit preparations and jams”, Trends in Food Science & Technology 16 (2005) 433–441, doi:10.1016/j.tifs.2005.07.001.

[5] Poliana M. Santos, “Detection and quantification of milk adulteration using time domain nuclear magnetic resonance (TD-NMR)” Microchemical Journal Volume 124, January 2016, Pages 15–19, doi:10.1016/j.microc.2015.07.013

[6] http://mehrashubham618.blogspot.com/2012/12/adultrance-in-food.html

[7] Mutia Nurulhusna Hussain, Mohd Fared Abdul Khir, Mohd Hafizulfika Hisham, And Zalhan Md Yusof, “Feasibility Study Of Detecting Canola Oil Adulteration With Palm Oil Using Nir Spectroscopy And Multivariate Analysis “, International Conference On Information, Communication Technology And System,2014.

[8] P. Kelina Sahaya Rajesh , C. Kumaravelu , A. Gopal , S. Suganthi , “Studies On Identification Of Medicinal Plant Variety Based On NIR Spectroscopy Using Plant Leaves “, IEEE 978-1-4673-2818-0/13/$31.00 ©2013 .

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