3-MCPD Esters in Edible Oils Current Knowledge

Transcription

1 ILSI SEA Region 6th Asian Conference on Food and Nutrition Safety (Nov 2012) 3-MCPD Esters in Edible Oils Current Knowledge Nuzul Amri Ibrahim, Muhd Roddy Ramli, Raznim Arni Abdul Razak, Siew Wai Lin, Ainie Kuntom and Kalanithi Nesaretnam Malaysian Palm Oil Board MPOB

2 Outline Introduction MPOB s Approach Laboratory scale Pilot plant scale Method of Analysis Refining Experiments Mitigation Actions Conclusion

3 Introduction 3-MCPD esters are formed during refining of oils and fats. Important issue among the edible oil and fat fraternity Strategies to mitigate the formation of the esters have to be efficient The tool for measurement of the amount has to be robust

4 Parameters Contributing factors based on reports by several researchers Chloride DAG FFA Temperature of deodorization

5 Our approach To evaluate possible factors responsible for the formation of 3-MCPD esters To suggest possible solutions/alternatives to minimise the formation of the esters Experiment Heat test: laboratory scale Refining: pilot plant scale

6 Heat test 260 C, vacuum 3-MCPD esters analysis

7 Pilot plant scale refining: 200 kg

8 Pilot-plant scale refining: Condition Parameter H 3 PO 4 (%) B/ clay(%) Modified Standard Deod temp( C) Duration(h)

9 3-MCPD esters Method of Analysis

10 Analytical methods available Method Analyte (bound) Short method description DGF CIII 18 (09) B 3-MCPD Alkaline / H+ and chloride Derivatization --- extraction, GC- MS BfR 'Method 8' 3-MCPD Acidic, neutralisation Derivatization --- extraction, GC- MS BfR 'Method 9 & 10' 3-MCPD Alkaline / H+ chloride free Derivatization --- extraction, GC- MS ADM 3-MCPD Glycidyl ester LC-MS/TOF

11 Summary of the method of analysis: Determination of 3-MCPD Fatty Acid Esters in Edible Oils and Fats by GC-MS Oil/fat sample Internal standard (d 5-3- MCPD) Acidic transesterification (H 2 SO 4 ) Neutralization Derivatization (PBA) GC-MS Analysis

12 GC-MSD Instrument

13 3-MCPD Esters Measurement Measurement of 3-MCPD esters by indirect method (Source: Matthaus, B. et. al.)

14 3-MCPD esters Method Performance and Results

15 Chromatogram

16 Calibration Curve

17 Method Performance Concentration (mg/kg), n = 6 % Recovery RSD (%) * CPO spiked with different 3-MCPD concentration levels, analyzed according to the sample extraction procedure

18 Heat test Results and discussion Effect of storage at ambient temperature Effect of FFA and DAG Effect of chloride Effect of rinsing CPO

19 Effect of storage DAG/F FFA/3-MCPDE DAG FFA 3-MCPDE Storage, weeks Condition: At ambient for 2 months Sampling: Weekly Drawn samples were heated to 260 C, 2 h

20 Effect of FFA MCPD DE, mg/kg FFA content, % C16

21 3-MCPDE levels in DAG oil Sample Feed oil (EIE) DAG oil Econa 3-MCPDE(ppm) Not detected

22 Mitigation Eliminate as much chlorides from CPO (At the mill purifier stage). Avoid using strong acid for degumming Try water degumming. For acid degumming, neutralise its effects if possible. Use neutral bleaching earth. Lower deodorisation temperature.

23 Conclusion Method of analysis Verification of the method showed that the % recovery of the spiked concentration levels falls within the acceptable range ( %) Linear calibration curve was established, with R LOD was optimized at 0.25 mg/kg (in 100mg sample) Formation of 3-MCPD esters Chloride content is the critical factor in the oil Eliminate as much chlorides from CPO DAG does not show strong correlation with the formation of 3- MCPD esters More on the formation of GE Acid the activating factor for high values 3-MCPD esters during refining

24 The team Acknowledgements Dr Kalanithi, Dr Ainie Kuntom, Dr Siew Wai Lin, Muhd. Roddy Ramli, Razali Ismail, Mohd Mokmin, Rabeah, Voon, Zaizuhana, Norazura and staff of High oleic pilot plant, Innovative group, FSCC Unit

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