JIPI
Skip to main content Skip to main navigation menu Skip to site footer

Analisis 3-Monokloro-1,2-Propanadiol (3-MCPD) Ester dalam Minyak Sawit dengan Instrumen Kromatografi Gas-Spektroskopi Massa

  • Hanifah Nuryani Lioe
  • Nancy Dewi Yuliana
  • Dias Indrasti
  • Yane Regiyana
  • Cony Arisya Putri
Keywords: 3-MCPD derivatization, 3-MCPD esters, GC-MS, palm oil, phenylboronic acid

Abstract

A group of components called as 3-monochloropropane-1,2-diol (3-MCPD) esters has been found in some vegetable oils, particularly palm oil. Analysis of these components needs GC-MS instrument to reach a low level detection, parts per billion or ppb level. An effort to validate the 3-MCPD esters analysis by GC-MS method (Weiβhaar method) using phenyl boronic acid (PBA) as a derivatizing agent and isotopic internal standard (IS) 3-MCPD-D5 followed by the determination of 3-MCPD in commercial palm oils has been conducted. The analytical results showed the instrumental performance as follows: instrument linearity for the analysis of 3-MCPD standard solutions containing IS 2.0 μg/mL was obtained at a concentration range of 0.25-7.50 μg/mL test solution with R2 higher than 0.990, precision of 3-MCPD as well as IS retention time was less than 2.0% which was acceptable according to JECFA guidance. Instrument detection limit (LOD) and limit of quantitation (LOQ) were read from GC-MS based on the linearity experiment, i.e. 0.17 and 0.59 μg/mL solution, respectively. Method linearity by using palm oil as a matrix also showed R2 higher than 0.990. Recovery test result at 40 μg/g gave an accuracy at 83.29 ± 7.12% which is in the range of AOAC standard (80-110%) and precision at 5.38% (less than RSDHORWITZ). Analysis of 14 palm oils from local market showed 100% of the sampels were positive to contain 3-MCPD esters. 3-MCPD esters in palm oil were found at a concentration range of 8.15-58.14 µg 3-MCPD/g sample.

Downloads

Download data is not yet available.

Author Biographies

Hanifah Nuryani Lioe
Departemen Ilmu dan Teknologi Pangan, Fakultas Teknologi Pertanian, Institut Pertanian Bogor, Kampus IPB Darmaga, Bogor 16680
Nancy Dewi Yuliana
Departemen Ilmu dan Teknologi Pangan, Fakultas Teknologi Pertanian, Institut Pertanian Bogor, Kampus IPB Darmaga, Bogor 16680
Dias Indrasti
Departemen Ilmu dan Teknologi Pangan, Fakultas Teknologi Pertanian, Institut Pertanian Bogor, Kampus IPB Darmaga, Bogor 16680
Yane Regiyana
Departemen Ilmu dan Teknologi Pangan, Fakultas Teknologi Pertanian, Institut Pertanian Bogor, Kampus IPB Darmaga, Bogor 16680
Cony Arisya Putri
Departemen Ilmu dan Teknologi Pangan, Fakultas Teknologi Pertanian, Institut Pertanian Bogor, Kampus IPB Darmaga, Bogor 16680

References

[AOAC] Association of Analytical Communities. 2012. AOAC Official Methods Of Analysis, Appendix K: Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals. Tersedia pada (Mei 2015): http://www.eoma.aoac.org/app_k.pdf

[BfR] Federal Institute for Risk Assessment. 2011. Collaborative study for the determination of 3-MCPD-fatty acid esters in edible fats and oils. Berlin: Germany. Tersedia pada: http://www.bfr.bund.de/cm/350/collaborative-study-for-the-determination-of-3-mcpd-fatty-acid-esters-in-edible-fats-and-oils.pdf

Cho W-S, Han BS, Nam KT, Park K, Choi M, Kim SH, Jeong J, Jang DD. 2008. Carcinogenicity study of 3-monochloropropane-1,2-diol in Sprague-Dawley rats. Food and Chemical Toxicology. 46(9): 3172-3177. http://doi.org/dptx5q

EURACHEM. 2014. The Fitness for Purpose of Analytical Methods: a Laboratory Guide to Method Validation and Related Topics. United Kingdom. Tersedia pada: https://www.eurachem.org/images/stories/Guides/pdf/MV_guide_2nd_ed_EN.pdf

Hamlet CG, Sadd PA. 2004. Chloropropanols and their esters in cereal products. Czech Journal of Food Sciences. 22: 259-262.

Hamlet CG, Asuncion L, Velíšek J, Doležal M, Zelinková Z, Crews C. 2011. Formation and occurrence of esters of 3-chloropropane-1,2-diol (3-CPD) in foods: What we know and what we assume. European Journal of Lipid Science and Technology. 113(3): 279-303. http://doi.org/ckmzq8

Harmita. 2004. Petunjuk Pelaksanaan Validasi Metode dan Perhitungannya. Majalah Ilmu Kefarmasian. 1(3): 117-135.

JECFA. 2006. Combined Compendium of Food Additives Specifications. Volume 4: Analytical methods, test procedures and laboratory solutions used by and referenced in the food additive specifications. Rome (IT): FAO. Tersedia pada: http://www.fao.org/docrep/009/a0691e/a0691e00.HTM.

Lanovia T, Andarwulan N, Hariyadi P. 2014. Validasi modifikasi metode Weiβhaar untuk analisis 3-MCPD ester dalam minyak goreng sawit. Jurnal Teknologi dan Industri Pangan. 25(2): 200-208.

Novelina YM, Sutanto, Fatimah A. 2009. Validasi Metode Analisis Penetapan Kadar Senyawa Siklamat Dalam Minuman Ringan. Jakarta (ID): Prodising PPI Standardisasi 2009. Tersedia pada: http://lib.bsn.go.id/index.php?/mjlh_artikel/majalah/detail_simple/584

Razak RAA, Kuntom A, Siew WL, Ibrahim NA, Ramli MR, Hussein R, Nesaretnam K. 2012. Detection and Monitoring of 3-monochloropropane-1,2-diol (3-MCPD) esters in cooking oils. Food Control. 25(1): 355-360. http://doi.org/btctnk

Rietjens IMCM, Scholz G, Berg I, Schilter B, Slob W. 2012. Refined hazard characterization of 3-MCPD using benchmark dose modeling. European Journal of Lipid Science and Technology. 114(10): 1140-1147.

Schilter B, Scholz G, Seefelder W. 2011. Fatty acid esters of chloropropanols and related compounds in food: Toxicological aspects. European Journal of Lipid Science and Technology. 113(3): 309-313. http://doi.org/c5s42q

Seefelder W, Varga N, Struder A, Williamson G, Scanlan FP, Stadler RH. 2008. Esters of 3-chlor-1,2-propanediol (3-MCPD) in vegetable oils: Significance in the formation of 3-MCPD. Food Additives and Contaminants. 25(4): 391-400. http://doi.org/cngmv8

Svejkovska B, Novotny O, Divinová V, Reblova Z, Dolezal M, Velíšek J. 2004. Esters of 3-Chloropropane-1,2-Diol in Foodstuffs. Czech Journal of Food Sciences. 22(5): 190-196.

Zelinková Z, Svejkovska B, Velíšek J, Doležal M. 2006. Fatty acid esters of 3-chloropropane-1,2-diol in edible oils. Food Additives and Contaminants. 23(12): 1290-1298. http://doi.org/fng54c

Weiβhaar R. 2008. Determination of total 3-chloropropane-1,2-diol (3-MCPD) in edible oils by cleavage of MCPD esters with sodium methoxide. European Journal of Lipid Science and Technology. 110(2): 183-186. http://doi.org/c5s4nr

Published
2015-08-26
How to Cite
Lioe, H. N., Yuliana, N. D., Indrasti, D., Regiyana, Y., & Putri, C. A. (2015). Analisis 3-Monokloro-1,2-Propanadiol (3-MCPD) Ester dalam Minyak Sawit dengan Instrumen Kromatografi Gas-Spektroskopi Massa. Jurnal Ilmu Pertanian Indonesia, 20(2), 115-123. https://doi.org/10.18343/jipi.20.2.115

Most read articles by the same author(s)

1 2 3 > >>