Characterization of virgin coconut oil and multiple instrument approach for the detection of lard adulteration in model virgin coconut oil
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(2) H. T. U. PM. CHARACTERIZATION OF VIRGIN COCONUT OIL AND MULTIPLE INSTRUMENT APPROACH FOR THE DETECTION OF LARD ADULTERATION IN MODEL VIRGIN COCONUT OIL. IG. By. ©. C. O. PY. R. TENGKU SALWANI BINTI TENGKU MANSOR. Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia, in Fulfilment of the Requirements for the Degree of Master of Science November 2011.
(3) DEDICATION. I dedicate this thesis to the 4 pillars of my life:. PM. 1) Mighty God Allah, who is always there to listen to my prayers. 2) My beloved husband, Dr Ahmad Syukri Jamaludin for all your patience and. U. love through sunshine and rain. 3) My beautiful son, Ahmad Suhayl for the joy you bring. H. T. 4) My parents and parents in laws for your unrelenting support. ©. C. O. PY. R. IG. Thank you very much for everything.
(4) Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfilment of the requirement for the degree of Masters of Science CHARACTERIZATION OF VIRGIN COCONUT OIL AND MULTIPLE INSTRUMENT APPROACH FOR THE DETECTION OF LARD ADULTERATION IN MODEL VIRGIN COCONUT OIL By. PM. TENGKU SALWANI BINTI TENGKU MANSOR. Chair: Professor Dato’ Yaakob Bin Che Man, PhD. T. Institute: Halal Products Research Institute. U. November 2011. H. The driving force for adulteration is to cut cost and to increase profit. However, in. IG. the case of adulteration using animal oils, this would also affect in terms of consumers beliefs and practice such as for Hindus, vegans and vegetarians, Jews and. R. Muslims. For Muslims, adulteration using lard (LD) or improperly slaughtered. PY. animal oils is of significant issue. Detecting adulteration in fats and oils especially the high-value oils such as virgin coconut oil (VCO) is indeed needed. The attempt to find the most effective, simple, chemical-free and straightforward analysis without. O. compromising the sensitivity and specificity is essential. Therefore, the overall. C. objective of this study is to apply these three instruments, namely differential scanning calorimeter (DSC), electronic nose/ fast gas-chromatography (fast GC) and. ©. Fourier transform infrared (FTIR) spectroscopy to detect LD adulterations in VCO. VCO is prepared through the ‘wet’ and ‘dry’ methods, while LD was rendered from adipose tissue of pig using microwave oven. In the first phase, the VCO samples were characterized and analyzed physicochemically. The results showed that in general all VCO samples conformed to the Asian and Pacific Coconut Community.
(5) (APCC, 2003) and does not differ strikingly from each other. Subsequently, samples of VCO and LD were mixed in different concentration (v/v). Each sample admixtures were subjected to analysis of fast GC, FTIR and DSC. Some chemical analyses were performed such as iodine value (IV) and peroxide value (PV). In addition, fatty acid. PM. (FA) and triacylglycerol (TAG) analyses were also conducted using gas chromatography-flame ionization detector (GC-FID) and high performance liquid. chromatography (HPLC), respectively, as the control experiments. Simple linear. U. regression on fast GC data demonstrated that three peaks on the fast GC. chromatogram were found to fit the second order polynomial curve with R2 of. T. 0.8121, 0.8349 and 0.9344, respectively. Partial least square (PLS) from FTIR. H. spectroscopy was able to predict LD adulteration in VCO with the equation y =. IG. 0.999x + 0.006. Meanwhile, DSC showed that Te A (endset peak A) in the endothermic curve and Tr D (temperature range for peak D) in the exothermic curve. R. were found to have good predictor ability in determining percentage LD adulteration. PY. in VCO with the equation from step 2 of stepwise multiple linear regression (SMLR); % LD adulteration = 293.1 – 11.36 (Te A) – 2.17 (Tr D) and R2 adjusted of 95.82. To conclude, all three techniques were able to detect LD in VCO with ease. ©. C. O. and without the use of chemicals..
(6) Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai memenuhi keperluan untuk ijazah Master Sains. PM. Oleh TENGKU SALWANI BINTI TENGKU MANSOR. U. November 2011. T. Pengerusi: Profesor Dato’ Yaakob Bin Che Man, PhD. H. Institut: Institut Penyelidikan Produk Halal. IG. Pendorong utama terhadap pencemaran dalam makanan adalah untuk mengurangkan kos dan meningkatkan keuntungan. Namun begitu, pencemaran lemak haiwan akan. R. menjejaskan amalan kepercayaan sesetengah penganut beragama Hindu, vegan dan. PY. ‘vegetarian’, penganut agama Yahudi dan juga Muslim. Bagi penganut Islam, penggunaan lemak khinzir (LK) ataupun penggunaan lemak haiwan yang tidak disembelih secara sah merupakan isu yang penting. Pengesanan pencemaran di. O. dalam lemak dan minyak terutamanya minyak yang bernilai tinggi seperti Minyak. C. Kelapa Dara (MKD) memang diperlukan. Percubaan untuk menemui teknik yang paling efektif, mudah dan tidak menggunakan bahan kimia tanpa mengurangkan. ©. sensitiviti dan spesifisiti adalah sangat-sangat diperlukan. Oleh itu, objektif keseluruhan kajian ini adalah untuk menggunakan Pembezaan Pengimbasan Kalorimeter (PPK), hidung elektronik/ Kromatografi-gas pantas (KG pantas) dan Pengubah Fourier Inframerah (PFIM) spektroskopi untuk mengesan kehadiran LK di dalam MKD. MKD telah disediakan melalui proses ‘kering’ dan ‘basah’, manakala.
(7) LK dihasilkan daripada ketuhar gelombang mikro. Pada fasa pertama, sampelsampel MKD ini dianalisa sifat fizikal dan kimianya dan didapati bahawa secara keseluruhannya semua MKD yang dihasilkan adalah mengikut kriteria yang diberikan oleh Persatuan Kelapa Asian dan Pasifik (APCC, 2003) dan tidak berbeza. PM. antara satu sama lain secara keterlaluan. Sampel-sampel MKD dan LK kemudiannya. dicampur dalam pelbagai kepekatan (v/v). Setiap sampel dianalisa oleh GK pantas, PFIM dan PPK. Analisis kimia juga telah dijalankan ke atas sampel-sampel ini. U. seperti nilai iodin dan nilai peroksida. Analisis asid lemak (AL) dan triasilgliserol. (TAG) juga dilakukan menggunakan kromatografi gas-pengesan pengionan nyala. T. (KG-PPN) dan juga Kromatografi Cecair Berprestasi Tinggi (KCBT) sebagai. H. eksperimen kawalan. Analisa Regresi Linear Mudah pada data KG pantas. IG. menunjukkan bahawa tiga puncak di kromatogram KG pantas serasi dengan lengkungan polinomial aturan kedua dengan R2 0.8121, 0.8349 dan 0.9344. Statistik. R. Persegi Separa Terkecil (PST) daripada PFIM juga dapat meramalkan LK di dalam. PY. MKD dengan persamaan matematik y = 0.999x + 0.006. Disamping itu, PPK menunjukkan bahawa Te A (suhu akhiran puncak A) dan Tr D (perbezaan suhu puncak D) pada keluk eksoterma dapat mengesan peratus LK di dalam MKD dengan. O. persamaan matematik daripada langkah kedua statistik Regresi Linear Berbilang. C. Langkah (RLBL); yakni % percampuran LK = 293.1 – 11.36 (Te A) – 2.17 (Tr D) dan penyesuaian R2 = 95.82. Sebagai kesimpulan, ketiga-tiga teknik ini berjaya untuk. ©. mengsan kehadiran LK di dalam MKD dengan mudah dan tanpa menggunakan bahan kimia..
(8) ACKNOWLEDGEMENTS. I would like to express my deepest appreciations and immense thanks to my Supervisor, Professor Dato’ Dr Yaakob Bin Che Man, whose support and guidance. PM. from the initial phase till the end has enabled me to learn something new and. U. valuable, as well as giving me insight to the understanding of the subject.. I am also greatly indebt to my Co-Supervisor, Associate Prof Dr Shuhaimi. T. Mustafa for his unremitting assistance, considerations and thoughtfulness towards. H. myself.. IG. Special thank to my colleagues especially Abdul Rohman for sharing your knowledge and expertise with me. Same goes to Nasyrah, Aisyah, Akasyah,. R. Sarafhana, Wan Farizan, Yanti, Aina, Nina, Azira, Irmie, Hanif, Shariena, Nadiha,. PY. Wan, Farihah, Ilyia, Dr Zuledham, Hazim and Ali, who would always be mentors to. O. me and for being there with me, be it rain or sunshine.. Lastly, I greatly appreciate Universiti Putra Malaysia for providing the funds. ©. C. for the study and to give me the chance to study here.. Thank you all..
(9) PM. I certify that a Thesis Examination Committee has met on 29th November 2011 to conduct the final examination of Tengku Salwani Binti Tengku Mansor on her thesis entitled “ ” 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 Masters of Science degree.. IG. H. Amin Ismail, PhD Professor Faculty of Medicine and Health Sciences Universiti Putra Malaysia (Internal Examiner). T. Professor Faculty of Food Science and Technology Universiti Putra Malaysia (Chairman). U. Members of the Thesis Examination Committee were as follows:. PY. R. Tan Chin Ping, PhD Associate Professor Faculty of Food Science and Technology Universiti Putra Malaysia (Internal Examiner). ©. C. O. Bahruddin Saad, PhD Professor School of Chemical Sciences Universiti Sains Malaysia 11800, Minden, Pulau Pinang Malaysia (External Examiner). ______________________ Professor and Deputy Dean School of Graduate Studies Universiti Putra Malaysia Date:.
(10) This thesis was submitted to the Senate of Universiti Putra Malaysia and has been accepted as fulfillment of the requirement for the degree of Masters of Science. The members of the Supervisory Committee were as follows:. PM. Yaakob Bin Che Man, PhD Professor Halal Products Research Institute Universiti Putra Malaysia (Chairman). U. Shuhaimi Bin Mustafa, PhD Associate Professor Halal Products Research Institute Universiti Putra Malaysia (Member). H. T. ______________________ BUJANG BIN KIM HUAT, PhD Professor and Dean School of Graduate Studies Universiti Putra Malaysia. ©. C. O. PY. R. IG. Date:.
(11) DECLARATION. U. PM. I declare that the thesis is my original work except for quotations and citations which have been duly acknowledged. I also declare that it has not been previously, and is not concurrently, submitted for any other degree at Universiti Putra Malaysia or at any other institution.. _______________________________. ©. C. O. PY. R. IG. H. T. TENGKU SALWANI BINTI TENGKU MANSOR Date: 29 November 2011.
(12) TABLE OF CONTENTS. !" iiii iv vi ix xi xv xvii xviii. U. PM. DEDICATION ABSTRACT ABSTRAK APPROVAL DECLARATION LIST OF TABLES LIST OF FIGURES LIST OF ABBREVIATIONS. T. CHAPTER GENERAL INTRODUCTION. 2. LITERATURE REVIEW 2.1 Virgin Coconut Oil 2.1.1 Methods of VCO extraction 2.1.2 Physicochemical characteristics 2.1.3 Benefits and uses 2.2 Lard 2.2.1 Physicochemical characteristics 2.2.2 Uses 2.3 Adulteration of Foods 2.3.1 Implications 2.3.2 Methods of detecting adulterations in food products 2.3.3 Lard adulterations 2.4 Electronic Nose/Fast Gas Chromatography (Fast GC) 2.4.1 Working steps 2.4.2 Fast GC – surface acoustic wave (SAW) sensor 2.4.3 Practical uses 2.4.4 Advantages and disadvantages 2.5 FTIR 2.5.1 Instrumentation and sample handling techniques. 2.5.2 IR spectra of oil 2.5.3 Advantages and disadvantages 2.6 DSC 2.6.1 DSC in fats and oils 2.6.2 Advantages and disadvantages. ©. C. O. PY. R. IG. H. 1. 1 5 5 6 9 9 12 13 16 17 18 19 23 26 29 29 31 32 32 33 34 36 36 38 40.
(13) PHYSICOCHEMICAL PROPERTIES OF VIRGIN COCONUT OIL EXTRACTED FROM DIFFERENT PROCESSING METHODS 3.1 Introduction 3.2 Materials and Methods 3.2.1 Materials 3.2.2 Extraction methods 3.2.3 Oil recovery 3.2.4 Physicochemical analyses 3.2.5 Fatty acid methyl esters (FAME) compositional analysis 3.2.6 Triacylglycerol (TAG) analysis by HPLC 3.2.7 Tocopherol analysis 3.2.8 Statistical analysis 3.3 Results and discussion 3.3.1 Oil Recovery 3.3.2 Physicochemical Analysis 3.3.3 Color 3.3.4 Fatty acid methyl esters (FAME) compositional analysis 3.3.5 TAG Analysis By Reverse Phase HPLC 3.3.6 Tocopherol Analysis by HPLC 3.4 Conclusions. 41 41 42 42 42 44 45. APPLICATION OF FAST GAS CHROMATOGRAPHY AND FOURIER TRANSFORM INFRARED SPECTROSCOPY FOR ANALYSIS OF LARD ADULTERATION IN VIRGIN COCONUT OIL 4.1 Introduction 4.2 Materials and Methods 4.2.1 Blends 4.2.2 Chemical analyses 4.2.3 Fast gas chromatography-surface acoustic wave (GC-SAW) detector system analysis 4.2.4 FTIR Spectroscopic analysis 4.2.5 Statistical Analysis 4.3 Results and Discussion 4.3.1 Chemical analysis 4.3.2 Fast gas chromatography-surface acoustic wave (GC-SAW) detector system analysis 4.3.3 FTIR analysis 4.4 Conclusions. ©. C. O. PY. 4. 46 47 47 48 48 48 51 54 55 58 60 63. R. IG. H. T. U. PM. 3. 64 64 66 67 67 67 68 69 69 69 71 77 81.
(14) EMPLOYMENT OF DIFFERENTIAL SCANNING CALORIMETER IN DETECTING LARD ADULTERATION IN VIRGIN COCONUT OIL 5.1 Introduction 5.2 Materials and Methods 5.2.1 Preparation of Blends 5.2.2 Chemical analyses 5.2.3 Fatty acid (FA) compositional analysis 5.2.4 Triacylglycerol (TAG) compositional analysis by HPLC 5.2.5 Thermal analysis by DSC 5.2.6 Statistical analysis 5.3 Results and Discussion 5.3.1 Chemical analysis 5.3.2 Fatty acid (FA) compositional analysis 5.3.3 TAG analysis by reverse-phase HPLC 5.3.4 Thermal analysis by DSC 5.4 Conclusions. 82 82 83 84 84 84. SUMMARY, GENERAL CONCLUSION AND RECOMMENDATION FOR FUTURE RESEARCH 6.1 Summary 6.2 General Conclusion 6.3 Recommendation for Future Research. R. IG. 6. H. T. U. PM. 5. ©. C. O. PY. REFERENCES BIODATA OF STUDENT LIST OF PUBLICATIONS. 84 85 85 86 86 87 91 98 111. 112 112 113 113 115 128 129.
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