Effects of Physical Structure and Surface Charge of Adsorbents for Reduction of Biogenic Amines in Salt-Fermented Fish Sauce
- Alternative Title
- 흡착제의 물리적 구조와 표면전하에 의한 액젓의 바이오제닉아민 저감 효과
- Abstract
- The purpose of this study is to efficiently reduce the large amount of BAs, which has been a continuous problem in salt-fermented fish sauce, while minimizing sensory reduction by using an adsorption method. In Chapter 1, the chemical quality and hygienic safety of domestic salt-fermented fish sauces (23 anchovy fish sauce, 24 sand lance fish sauce, 12 seasoned fish sauce, and 9 sauce-type fish sauce) were evaluated to verify whether they met domestic (Korea) standards and CODEX standard. As a result of the analysis, most of the standard for pH, moisture, TN, AN, salinity, and microorganisms were suitable, and no serious problems were found. However, the histamine content of anchovy fish sauce products was 18.65-1574.44 mg/kg and sand lance fish sauce products were 4.56-760.83 mg/kg, and only 17% and 54% of the products met CODEX standards (400 mg/kg), respectively. In addition, the content of other BAs was also significantly higher than previously reported, confirming the need for BAs reduction technology.
In Chapter 2, 10 types of adsorbents (talc, kaolin, clay acid, bentonite, diatomite, zeolite, 4 types of activated carbon) were used to develop a reduction technique that could selectively remove BAs from salt-fermented fish sauce at the final stage of the product and has no sensory effect. As a result of the analysis, adsorbents except activated carbon have no significant effect on color, pH, AN, BAs, and volatile compounds of salt-fermented fish sauce. On the other hand, activated carbons significantly reduced BAs (maximum TRP 100%, PEA 92%, CAD 17%, HIS 42%, and TYR 87%) and negligibly reduced AN up to 3%. In addition, most of the volatile components were reduced, but the flavor was sensually improved. These results showed that different types of activated carbons have different effects on salt-fermented fish sauce, and it served as an opportunity to suggest an interaction mechanism between anchovy fish sauce and activated carbon using the differences found.
In Chapter 3, the characteristics of activated carbon were analyzed using FE-SEM, Boehm's titration method, point of zero charge, zeta potential, FT-IR, and XPS, and based on these characteristics, the interaction mechanism between anchovy fish sauce and activated carbon was explained. The acid-modified AC-A and AC-B have rough surfaces, high total acidity, low pHpzc, rich surface functional groups, and zeta potential value of around -10 mV at the pH of salt-fermented fish sauce. On the other hand, AC-C has smooth surface, low total acidity, high pHpzc, poor surface functional groups, and zeta potential value greater than -30 mV at all pHs. These characteristics can explain why the AN reduction rate of activated carbons are generally low regardless of the type, and why AC-C has higher histamine reduction and less color reduction despite its lower surface area compared to other activated carbons.
In Chapter 4, an optimal condition was found using response surface analysis with independent variables set based on the mechanism, and based on this condition, a two-stage adsorption method was developed to maximize BAs reduction and applied to the industry. The optimal amount of adsorbent was AC-C 2% and diatomite 0.9%, and the optimal reaction condition was 27℃ and 97 min. When the optimal conditions were industrially transformed and applied to the two-stage adsorption method, maximum TRP, PHE 100%, CAD 10%, HIS 61%, and TYR 96% were reduced, whereas the reduction rates of AN, TN, free amino acid related to taste and color were very small. Afterwards, when produced using the two-stage adsorption method in the factory, the same results as the laboratory scale were obtained, confirming the possibility of industrialization of BAs-reduced salt-fermented fish sauce.
The BAs reduction technology developed through this study can of course be used in the liquid food industry and can be easily applied in the salt-fermented fish sauce industry, which is mostly small businesses. It is also expected that this will increase the market size of the domestic salt-fermented fish sauce industry by expanding exports, and that it will be able to take responsibility for the safety of citizens by standardizing salt-fermented fish sauce that is indiscriminately distributed in Korea where there is no BAs standard.
- Issued Date
- 2023
- Awarded Date
- 2023-02
- Type
- Dissertation
- Publisher
- 부경대학교
- Alternative Author(s)
- 인정진
- Affiliation
- Pukyong National University, Graduate School
- Department
- 대학원 식품공학과
- Advisor
- 심길보
- Table Of Contents
- Chapter1. Monitoring of commercial salt-fermented fish sauce 1
1.1. Introduction 2
1.2. Materials and methods 7
1.2.1. Sample preparation 7
1.2.2. Reagents & chemicals 7
1.2.3. Solid content & pH 8
1.2.4. Salinity 8
1.2.5. Total nitrogen (TN) & amino nitrogen (AN) 9
1.2.6. Biogenic amines (BAs) 9
1.2.7. Microbiological contamination 15
1.2.7.1. Viable cell counts 15
1.2.7.2. Escherichia Coli & Total Coliforms counts 15
1.2.7.3. Vibrio parahaemolyticus & Staphylococcus aureus counts 15
1.3. Results and discussion 16
1.3.1. Solid content & pH 16
1.3.2. Salinity 19
1.3.3. TN & AN 21
1.3.4. BAs 28
1.3.5. Microbiological contamination 37
Chapter2. Effect of adsorbent treatment to reduce biogenic amines in anchovy fish sauce 42
2.1. Introduction 43
2.2. Materials and methods 48
2.2.1. Sample preparation 48
2.2.2. Particle size analysis (PSA) 50
2.2.3. Brunauer-Emmett-Teller (BET) 50
2.2.4. Color, pH & yield 51
2.2.5. AN & BAs 51
2.2.6. Volatile compounds (SPME-GC-MS) 51
2.2.7. Statistical analysis 53
2.3. Results and discussion 55
2.3.1. Physical properties of adsorbents 55
2.3.2. Color 59
2.3.3. pH, yield & AN 62
2.3.4. BAs 64
2.3.5. Volatile compounds 68
Chapter3. Interaction mechanism between salt-fermented fish sauce and activated carbon 82
3.1. Introduction 83
3.2. Materials and methods 85
3.2.1. Sample preparation 85
3.2.2. Field Emission Scanning Electron Microscope (FE-SEM) 85
3.2.3. Total acidity & basicity 86
3.2.4. Point of zero charge (pHpzc) 87
3.2.5. Zeta-potential 87
3.2.6. Fourier transform infrared spectroscopy (FT-IR) 88
3.2.7. X-ray photoelectron spectroscopy (XPS) 88
3.3. Results and discussion 88
3.3.1. SEM-EDS 88
3.3.2. Total acidity & basicity 93
3.3.3. pHpzc & Zeta-potential 95
3.3.4. FT-IR 97
3.3.5. XPS 100
3.3.6. Interaction mechanism between salt-fermented fish sauce and activated carbon 104
Chapter4. Optimization of activated carbon treatment in anchovy fish sauce using response surface methodology & design of two-stage adsorption method for industrialization 111
4.1. Introduction 112
4.2. Materials and methods 114
4.2.1. Materials 114
4.2.1.1. Response surface methodology (RSM) sample preparation 114
4.2.1.2. Two-stage adsorption treated sample preparation in laboratory 114
4.2.1.3. Two-stage adsorption treated sample preparation in industry 115
4.2.2. RSM 117
4.2.3. Proximate composition 121
4.2.4. pH, color & salinity 121
4.2.5. Volatile basic nitrogen (VBN) 121
4.2.6. AN & BAs 122
4.2.7. Free amino acids 122
4.2.8. Volatile compounds 123
4.2.9. Statistical analysis 123
4.3. Results and discussion 123
4.3.1. Effect of activated carbon and diatomite content on anchovy fish sauce during adsorption treatment 123
4.3.2. Effect of temperature and time on anchovy fish sauce during adsorption treatment 142
4.3.3. Proximate composition 161
4.3.4. Physicochemical changes of anchovy fish sauce produced by two-stage adsorption method in laboratory scale 161
4.3.4.1. Color 161
4.3.4.2. Salinity, VBN, TN & AN 163
4.3.4.3. Free amino acids 165
4.3.4.4. BAs 168
4.3.4.5. Volatile compounds 170
4.3.5. BAs & AN of salt-fermented fish sauce produced by two-stage adsorption method in industrial scale 177
5. Conclusions 181
6. References 184
Abstract (In Korean) 201
- Degree
- Master
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