UNIVERSITI PUTRA MALAYSIA. DEVELOPMENT OF BULK PACKAGING AND STORAGE OF SHALLOT (Allium ascalonium) PUREE NOOR AZIZAH BINTI AHMAD FSMB

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UNIVERSITI PUTRA MALAYSIA DEVELOPMENT OF BULK PACKAGING AND STORAGE OF SHALLOT (Allium ascalonium) PUREE NOOR AZIZAH BINTI AHMAD FSMB 2008 14

DEVELOPMENT OF BULK PACKAGING AND STORAGE OF SHALLOT (Allium ascalonium) PUREE BY NOOR AZIZAH BINTI AHMAD Tbesis Submitted to tbe Scbool of Graduate Studies, Universiti Putra Malaysia, in Fulfilment of tbe Requirement for tbe Degree of Master of Science. December 2008

Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfilment of the requirement for the degree of Master of Science. DEVELOPMENT OF BULK PACKAGING AND STORAGE OF SHALLOT (Allium ascalonium) PUREE By NOOR AZIZAB BINTI AHMAD December 2008 Chairman : Professor Russly Abdul Rahman, PhD Faculty : Food Science and Technology The present trend where modern housewives have limited time in preparing food and also the food industry and services need ingredients in convenience form in order to cut down extensive labour, has led to the increase of ready to use food ingredient. With this in mind, ready to use shallots (Allium asea/onium) is able to satisfy the needs of retail and institutional consumers. Studies on physico-chemical changes, microbiological test and sensory evaluation for development of processing treatments of shallot puree using mild heat and acidification were carried out. The L value (L*) and hue angle (Hab) of shallot puree increased significantly (p<o.05) during 8 weeks storage at 5±1 C (85-95% RH), whilst, the chroma value (C*) decreased significantly (p<o.05). Total plate count (TPC) slowly increased during 11

storage period in all samples. The yeast and mould count increased in both acidified and control samples, whilst, the increment of coliforms was only detected in control sample. However, the mean scores on colour, odour and overall acceptability decreased significantly (p<o.os) during storage period for all samples. Total soluble solid (TSS) and ph value slowly decreased during storage period. Sample that was acidified + heated could be kept for 8 weeks at S± 1 C (85-9S% RH) followed by 7 weeks for acidified sample. The shelf life of less than 2 weeks was obtained for both heated and control samples. The optimal conditions of modified atmosphere storage were investigated, in order to provide a basis for the development of modified atmosphere packs for shallot puree. Qualities of shallot puree were tested at different atmospheric condition (with or without S, 10, IS and 20 % CO2) and temperatures (S, IS and 2S) ±1 C by using OnylLLDPE and PET /PEl A1IPE as packaging materials. The carbon dioxide content in shallot puree packed with OnylLLDPE decreased significantly (p<0.05) for all treatments during 12 weeks of storage, whilst the oxygen content increased significantly (p<o.os). The L value (L*) and hue angle (Hat,) showed significant (p<0.05) increased in all samples: However, the chroma value (C*) and organoleptic evaluation decreased significantly (p<o.os) throughout the storage period. TPC and Lactobacillus spp. count increased slowly during storage period in all samples. However, the population of coliform, yeast and mould count and Pseudomonas spp. count were undetected in all samples. The ph value and TSS decreased significantly 111

(p<0.05) in shallot puree packed with different carbon dioxide contents and packaging materials during storage period. Shallot puree packed in OnyILLDPE with 10% carbon dioxide was found to be the best treatment for extending the storage life up to 12 weeks at 5±1 C (85-95% RH). The quality changes of shallot puree stored at 10 % C02 and packed in OnylLLDPE was studied in bulk form through out storage. There was a significant (p<0.05) increase in the L value (L*) and hue angle (Bab) but not in chroma value (C*) (p<o.05) for both treatments. There is a highly significant decrease (p<0.05) in sugar (fiuctose, glucose and sucrose) content of shallot puree throughout storage, whilst, total sugar showed no significant (p>0.05) difference between treatments during storage. Volatile oil of shallot puree contained sulphur group as major compounds. TPC and Lactobacillus spp. count gradually increased until the end of storage period. IV

Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai memenuhi keperluan untuk ijazah Master Sains. PERKEMBANGAN PEMBUNGKUSAN PUKAL DAN PENY PANAN PURl BA WANG MERAB (AQi"m ascajoni"m) Oleh NOOR AZIZAH BINTI AHMAD Disember 2008 Pengerusi : Profesor Russly Abdul Rahman, PhD Fakulti : Sains dan Teknologi Makanan Gaya hidup moden di mana para suri rumah yang kesuntukan masa untuk menyediakan makanan. dan juga dalam perkhidmatan dan industri makanan yang memerlukan bahan atau ramuan dalam bentuk yang mudah disediakan bagi mengurangkan pekerja menyebabkan ianya menjadikan faktor penting untuk meningkatkan penghasilan ramuan makanan yang sedia digunakan. Dengan mengambil kira faktor tersebut, bawang merah yang sedia digunakan adalah berupaya untuk memenuhi keperluan pelanggan jualan runcit dan institusi. Kajian ke atas perubahan-perubahan fiziko-kimia, ujian mikrobiologikal dan penilaian ujirasa bagi pembangunan perlakuan pemprosesan purl bawang merah (Allium ascalonium) menggunakan pemanasan sederhana dan pengasidan telah dijalankan. v

Nilai L (L*) dan hue angle <Hat,) puri bawang menunjukkan peningkatan yang sangat bererti (p<0.05) selama 8 minggu penyimpanan pada suhu 5±1 C (85-95% RH), manakala nilai chroma (C*) menurun dengan berkesan (p<0.05). Jumlah kiraan plat (TPC) bagi semua sampel telah meningkat secara perlahan-iahan semasa penyimpanan. Kiraan yis dan kulat pula didapati meningkat pada sampel yang diberi perlakuan pengasidan dan juga kawalan, manakala peningkatan bakteria kolifom semasa penyimpanan hanya dapat dilihat pada sampel kawalan sahaja. Walau bagaimanapun, penilaian organoleptik telah menurun dengan sangat bererti (p<0.05) semasa tempoh penyimpanan bagi semua sampel. Jumlah pepejal lamt (TSS) dan nilai ph pula telah menurun secara perlahan semasa tempoh penyimpanan. Sampel yang diberi perlakuan asid + haba boleh disimpan selama 8 minggu pada suhu 5±1 C (85-95% RH) dan diikuti selama 7 minggu untuk sampel yang hanya diberi perlakuan asid sahaja. Manakala sampel yang diberi perlakuan haba sahaja dan sampel kawalan mempunyai tempoh penyimpanan kurang dari 2 minggu. Kondisi penylmpanan atmosfera terubahsuai yang optima telah dikaji untuk dijadikan asas terhadap pembangunan pembungkusan puri bawang merah secara atmosfera terubahsuai. Kualiti puri bawang merah telah diuji dalam keadaan atmosfera (tanpa atau dengan kehadiran kepekatan sebanyak 5, 10, 15 dan 20 peratus kandungan gas karbon dioksida) dan suhu (5, 15 dan 25) ±1 C yang berbeza dengan menggunakan OnylLLDPE dan PET/PE/AlIPE sebagai bahan pembungkus. Penurunan nilai kandungan gas karbon dioksida menunjukkan perbezaan bererti VI

(p<o.05) dalam puri bawang merah yang dibungkus dalam OnylLLDPE bagi semua perlakuan semasa tempoh 12 minggu penyimpanan, manakala nilai kandungan gas oksigen pula didapati meningkat dengan sangat bererti (p<o.05). Nilai L (L*) dan hue angle (Hat,) pula menunjukkan peningkatan yang sangat bererti (p<o.05) bagi semua perlakuan. Walau bagaimanapun, nilai chroma (C*) dan penilaian organoleptik menunjukkan penurunan yang sangat bererti (p<o.05) semasa penyimpanan. Jumlah kiraan plat (TPC) dan kiraan Lactobacillus spp. meningkat secara perlahan semasa penyimpanan bagi semua perlakuan. Walau bagaimanapun, bakteria kolifom, kiraan yis dan kulat serta kiraan Pseudomonas spp. tidak dapat dikesan pada semua sampel. Kandungan ph dan TSS telah menunjukkan perbezaan penurunan yang sangat bererti (p<0.05) dalam puri bawang merah yang dibungkus dengan kandungan gas karbon dioksida dan bahan pembungkusan yang berbeza semasa tempoh penyimpanan. Puri bawang merah yang dibungkus menggunakan komposisis kandungan gas 10010 karbon dioksida dalam OnylLLDPE didapati telah memberi kesan perlakuan yang paling baik untuk memanjangkan hayat simpanan selama 12 minggu pada suhu 5±1 C (85-95% RH). Perubahan mutu puri bawang merah yang disimpan dalam kandungan 10% karbon dioksida dan dibungkus dalam OnylLLDPE telah dikaji dalam bentuk pukal sepanjang penyimpanan. Nilai L (L *) dan hue angle (Hab) menunjukkan peningkatan yang sangat bererti (p<o.05) tetapi nilai chroma (C*) pula menurun dengan sangat bererti (p<0.05) bagi kedua-dua perlakuan semasa penyimpanan. Kandungan gula (fruktosa, glukosa dan sukrosa) dalam puri bawang telah menurun dengan sangat bererti (p<0.05) bagi kedua-dua VlI

perlakuan, manakala jumlah kandungan gula menunjukkan tiada perbezaan bererti (p>o.05) diantara perjakuan semasa penyimpanan. Sebatian minyak meruap di dalam puri bawang merah telah menunjukkan bahawa sebahagian besarnya adalah terdiri dari kumpulan sulfur. lumlah kiraan plat (TPC) dan kiraan Lactobacillus spp. pula meningkat secara perjahan sehingga akhir tempoh penyimpanan. Vlll

ACKNOWLEDGEMENTS Alhamdulillah, first of all I would like to express my utmost thanks and gratitude to Almighty Allah S.W.T who has given me the capability to complete this project and my salawat and salam to His righteous messenger, prophet Muhammad s.a.w. I would like to take this opportunity to express my appreciation and gratitude to the Chairman of my Supervisory Committee, Prof Dr. Russly Abd Rahman for his invaluable suggestion, guidance, discussion and patience throughout this project. I am also very grateful to the other members of supervisory committee, Prof Dr. Azizah Osman and Prof Dr. Salmah Yusof for their advices, encouragements and constructive comments towards the preparation of this thesis. My sincere gratitude is also extended to the financial support provided by the IRP A fund for this research, which was awarded to me. I am much indebted to Deputy Director and all the staff of the Packaging and Handling Programme, Food Technology Research Centre MARDI for their generous cooperation. Acknowledgement is also due to all my friends and also laboratory assistants who had given me the moral encouragement and support to complete my graduate study. Finally, I also wish to express my deepest appreciation to my beloved husband, Razali Mustaffa and daughters, Nurul Shazwani, Nurul Athirah Aimi and Nurul IX

Hana Alisya who have given me encouragement and support in one way or another during the many years of my seemingly never ending pursue for knowledge. I wish for every bead of sweat they produced will be in Allah's barakah. All from Allah and all back to Allah again. x

I certify that a Thesis Examination Committee has met on 21 December 2008 to conduct the final examination of Noor Azizah binti Ahmad on her thesis entitled "Development of Bulk Packaging and Storage of Shallot (Allium ascalonium) Puree" in accordance with the Universities and University Colleges Act 1971 and the Constitution of the Universiti Putra Malaysia [P.U.(A) 106] 15 March 1998. The Committee recommends that the student be awarded the Master of Science. Members of the Thesis Examination Committee were as follows: Yaakob Che Man, PhD Professor Institut Penyelidikan Produk Halal Universiti Putra Malaysia (Chairman) Roselina Karim, PhD Lecturer Faculty of Food Science and Technology Universiti Putra Malaysia (Internal Examiner) Abdulkarim Sabo Mohammed, PhD Lecturer Faculty of Food Science and Technology Universiti Putra Malaysia (Internal Examiner) Azhar Mat Easa, PhD Associate Professor School ofindustrial Technology Universiti Sains Malaysia (External Examiner) HUAT,PhD Professor and Deputy Dean School of Gr duate Studies Universiti Putra Malaysia Date: 28 April 2009 Xl

This thesis was submitted to the Senate of Universiti Putra Malaysia and has been accepted as fulfilment of the requirement for the degree of Master of Science. The members of the Supervisory Committee were as follows: Russly Abdul Rahman, PhD Professor Faculty of Food Science and Technology Universiti Putra Malaysia (Chairman) Azizah Osman, PhD Professor Faculty of Food Science and Technology Universiti Putra Malaysia (Member) Salmah Yusor, PhD Professor Faculty of Science and Technology Universiti Sains Islam Malaysia (Member) Professor an.""' 1 School of Graduate tudies Universiti Putra Malaysia I, PhD Date: 14 May 2009 xu

DECLARATION I declare that the thesis is my original work except for quotations and citations which have been duly acknowledged. I also declare that is has not been previously, and is not concurrently submitted for any other degree at UPM or at any other institution. NOOR AZIZAH BINTI AHMAD Date: 24 April 2009 Xlii

TABLE OF CONTENT Page ABSTRACT ABSTRAK ACKNOWLEDGEMENT APPROVAL DECLARATION LIST OF TABLES LIST OF FIGURES LIST OF SYMBOLS AND ABBREVIATIONS 11 V IX XI XlII XIX XXII XXIV CHAPTER 1 GENERAL INTRODUCTION 1 2 LITERATURE REVIEW History of Shallot Flavour Compound Antimicrobial Activity Other Chemical Constituents Shallot Puree Modified Atmosphere Packaging (MAP) Effect of the MAP on the Microbiological, Chemical, Biochemical, and Physical Properties of Foods MAP Gases Carbon Dioxide 4 4 7 9 11 13 14 16 19 19 XIV

Nitrogen Oxygen Gas Mixture Packaging Materials for MAP Foods Polyamide (PA) Polyethylene (PE) Polypropylene (PP) Polyethylene Terephthalate (polyester or PET) Storage Temperature of MAP Product Bulk Packaging System Bag-In-Box Corrugated Fibreboard Boxes 20 21 22 24 24 26 27 28 29 30 31 32 3 ESTABLISHMENT OF PROCESSING PARAMETERS FOR PRODUCTION OF SBALWT (Allium asea/onium) PUREE DURING STORAGE Introduction Materials and Methods Pre p aration of Puree Processing Treatments Packaging and Storage Sensory Evaluation 3S 36 36 37 37 38 xv

Determination of Colour Determination of ph Determination of Total Soluble Solids (TSS) Microbiological Analysis Statistical Analyses Results and Discussion Organoleptic Evaluation Colour Measurement Microbiological Analysis ph Va]ue Total Soluble Solids Content Conclusion 39 39 39 40 40 41 41 46 49 53 53 55 4 EFFECTS OF MODIFIED ATMOSPHERE PACKAGING ON STORAGE QUALITY OF SHALLOT (Allium ascalonium) PUREE Introduction Materials and Methods Preparation of Product Sampling Gas Analysis Packaging Material Permeability Sensory Evaluation 57 59 59 59 60 61 63 XVI

Determination of Colour Microbiological Analysis Determination of ph Determination of Total Soluble Solids (TSS) Results and Discussion Gases Concentration Sensory Evaluation Colour Measurement Microbiological Test Total Plate Count (TPC) Lactobacillus spp. Count Other Microorganisms ph Value Total Soluble Solid Content Conclusion 63 64 65 65 65 65 70 76 82 82 86 90 91 93 95 5 EFFECT OF BULK PACKAGING ON STORAGE QUALITY OF SHALLOT (Allium ascalollium) PUREE Introduction Materials and Methods Preparation of Puree 96 97 97 XVII

Sampling Determination of Colour Extraction and Determination of Sugar Profiles Extraction and Analysis of Volatile Compound Microbiological Analyses Results and Discussion Changes in Colour Changes in Sugar Content Volatile Compound Microbiological Test Conclusion 97 98 98 99 100 100 100 105 III 115 120 6 CONCLUSION AND RECOMMENDATIONS General Conclusions Recommendations 121 122 REFERENCES APPENDICES BIODATA OF STUDENT 124 140 184 XVllI

LIST OF TABLES Table Page 1 Flavour precursors detected in edible Alliums 9 2 Antibacterial activity of essential oil extracts of Allium plants against Staphylococcus aureus after 48 h 10 3 Antibacterial activity of essential oil extracts of Allium plants against Salmonella Enteritidis after 48 h 11 4 Nutrient composition of edible portion 12 5 Oxygen requirements of some microorganisms of relevance in modified atmosphere packaging 17 6 Sensivity of microorganisms relevant to modified atmosphere packaging to carbon dioxide 18 7 Recommended gas mixtures of MAP product 23 8 Common forms of corrugated fiberboard 34 9 Effect of different processing treatments on sensory evaluation 43 (colour) of shallot puree during chill storage 10 Effect of different processing treatments on sensory evaluation (odour) of shallot puree during chill storage 44 11 Effect of different processing treatments on sensory evaluation (ovej acceptability) of shallot puree during chill storage 45 12 Effect of different processing treatments on yeast and mould count (CFU g- l ) of shallot puree during chill storage 51 13 Effect of different processing treatments on coliforms count (MPNg- 1 ) of shallot puree during chill storage 52 14 Effect of modified atmosphere packaging (MAP) with different packaging materials on CO2 concentration (%) of shallot puree stored at 5± 1 C for 12 weeks 67 XiX

15 Effect of modified atmosphere packaging (MAP) with different packaging materials on 02 concentration (%) of shallot puree stored at 5± 1 C for 12 weeks 69 16 Effect of modified atmosphere packaging (MAP) with different packaging materials on colour acceptability of shallot puree stored at 5± 1 C for 12 weeks 71 17 Effect of modified atmosphere packaging (MAP) with different packaging materials on odour acceptability of shallot puree stored at 5±1 C for 12 weeks 74 18 Effect of modified atmosphere packaging (MAP) with different packaging materials on overall acceptability of shallot puree stored at 5± 1 C for 12 weeks 75 19 Effect of modified atmosphere packaging (MAP) with different packaging materials on L * value of shallot puree stored at 5±1 C for 12 weeks 79 20 Effect of modified atmosphere packaging (MAP) with different packaging materials on Hue angle of shallot puree stored at 5±1 C for 12 weeks 80 21 Effect of modified atmosphere packaging (MAP) with different packaging materials on chroma value of shallot puree stored at 5±1 C for 12 weeks 81 22 Effect of modified atmosphere packaging (MAP) with different packaging materials on total plate count (CFU g- I ) of shallot puree stored at 5± 1 C for 12 weeks 83 23 Effect of modified atmosphere packaging (MAP) with different packaging materials on Lactobacillus count (CFU g- l ) of shallot puree stored at 5± 1 C for 12 weeks 88 24 Effect of modified atmosphere packaging (MAP) with different packaging materials on ph value of shallot puree stored at 5± 1 C for 12 weeks 92 25 Effect of modified atmosphere packaging (MAP) with different packaging materials on total soluble solids content (OBrix) of shallot puree stored at 5± 1 C for 12 weeks 94 xx

26 27 Volatile oil compounds present in untreated (control) shallot puree stored at s± 1 C Volatile oil compounds present in shallot puree treated with 10% CO2 stored at S±I C 112 113 XXI

LIST OF FIGURES Figure Page 1 Effect of different processing treatments on colour changes (L * value) of shallot puree during chill storage 47 2 Effect of different processing treatments on colour changes (expressed in chroma value) of shallot puree during chill storage 48 3 Effect of different processing treatments on colour changes (expressed in hue angle) of shallot puree during chin storage 48 4 Effect of different processing treatments on total plate count (TPC) of shallot puree during chill storage 50 5 Effect of different processing treatments on ph value of shallot puree during chill storage 54 6 Effect of different processing treatments on total soluble solids of shallot puree during chill storage 55 7 L value of control and 10010 CO2 OnyILLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks. 101 8 Chroma value of control and 10% C02 OnyILLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 102 9 Hue angle of control and 10% C02 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 103 10 Fructose content of control and 100/ 0 CO2 OnylLLDPE packaging sha110t puree during storage at 5± 1 C for 12 weeks 106 11 Glucose content of control and 10010 C02 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 107 12 Sucrose content of control and 10% C02 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 109 XXll

13 Total sugar content of control and 10010 CO2 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 110 14 GeMS chromatogram of extracted volatile oil compound In control shallot puree stored at 5± 1 C 116 15 GeMS chromatogram of extracted volatile oil compound In treated shallot puree stored at 5± 1 C 117 16 Total plate count of control and 10% CO2 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 118 17 Lactobacillus spp. count of control and 10010 C02 OnylLLDPE packaging shallot puree during storage at 5± 1 C for 12 weeks 119 XXJlJ

LIST OF SYMBOLS AND ABBREVIATIONS BC % < > JlL BGP cc CFU cm C02 C02TR EMA EVOH g G/p GTR h HOPE Hg IU kg kgy kpa m Before Century Percent Less than More than Micro liter Micron Degree Celcius Bulk Gas pack Centimeter Cubic Colony Forming Unit Centimeter Carbon dioxide Carbon dioxide Transmission Rate Equilibrium Modified Atmosphere Ethyl Vinyl Alcohol Gram Ratio volume of gas and volume of product Gas Transmission Rate Hour High Density Polyethylene Mercury International Unit Kilogram Kilo gay Kilo Pascal Liter Meter XXIV