Sains Malaysiana 43(3)(2014): 407–413

Development and Validation of Gas Chromatography-Mass Spectrometric Method for the Determination of Epoxidized Soybean Oil in Foods Stored in Glass Jars with Metal Lids

(Pembangunan dan Validasi Kaedah Kromatografi Gas-Spektrometri Jisim bagi Penentuan

Minyak Kacang Soya Terepoksi dalam Makanan yang Disimpan di dalam Balang Kaca

Berpenutup Logam)

HONG KEAT QUEK¹, MOHD MARSIN SANAGI*^{1 2}, WAN AINI WAN IBRAHIM¹,

SYAIRAH SALLEH¹& MAZIDATULAKMAM MISKAM^{1 2}

¹Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia

81310 UTM Johor Bahru, Johor, Malaysia

²Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia

81310 UTM Johor Bahru, Johor, Malaysia

Received: 28 June 2012/Accepted: 6 July 2013

ABSTRACT

A method has been developed for the determination of epoxidized soybean oil (ESBO) in oily foods stored in glass jars with metal lids using gas chromatography-mass spectrometry (GC-MS). ESBO and its internal standard (cis,cis-11,12;14,15-diepoxyeicosanoate) were isolated from the matrix by transesterification process. The developed method showed good linear dynamic range between 0.7-20 μg mL-1 with coefficients of determination (R2) > 0.9968 and acceptable limit of detection and limit of quantitation of 7 and 23 mg kg-1, respectively, based on linearity calculations. Analyte recoveries were 90.84±27.24% for low concentration, 78.05±11.59% for medium concentration and 99.23±10.20% for high concentration. This first fully validated GC-MS method was successfully applied for the determination of ESBO in foods stored in glass jar with metal lid. Among the 31 food samples studied, 6 samples were found to exceed the specific migration limit of 60 mg kg-1 (based on EU Directive 2002/72/EC). The developed method is thus potentially useful for routine analysis for the determination of ESBO.

Keywords: Epoxidized soybean oil; foods stored in glass jars with metal lids; gas chromatography-mass spectrometry

ABSTRAK

Satu kaedah telah dibangunkan untuk menguji minyak kacang soya terepoksi (ESBO) dalam makanan berminyak di dalam balang kaca berpenutup logam menggunakan kromatografi gas-spektrometri jisim (GC-MS). ESBO dan piawai dalaman (cis,cis-11,12;14,15-diepoxyeicosanoate) telah dipisahkan daripada matrik menggunakan proses transesterifikasi. Kaedah yang dibangunkan ini menunjukkan dinamik linear yang baik antara 0.7-20 μg mL-1 dengan pekali penentuan (R2) > 0.9968 dan had pengesanan serta had kuantifikasi yang boleh diterima iaitu 7 dan 23 mg kg-1, masing-masing berdasarkan kepada pengiraan lineariti. Peratus pengembalian analit ialah 90.84±27.24%, bagi kepekatan rendah, 78.05±11.59% bagi kepekatan sederhana dan 99.23±10.20% bagi kepekatan tinggi. Kaedah GC-MS yang telah divalidasi sepenuhnya buat pertama kali telah berjaya diaplikasikan untuk penentuan ESBO dalam makanan yang disimpan di dalam balang kaca berpenutup logam. Daripada 31 sampel yang telah dikaji, 6 sampel didapati melebihi had 60 mg kg-1 mengikut undang-undang Eropah (EU Directive 2002/72/EC). Oleh itu, kaedah ini berpotensi untuk digunakan sebagai analisis rutin untuk penentuan ESBO.

Kata kunci: Kromatografi gas-spektrometri jisim; makanan disimpan di dalam balang kaca berpenutup logam; minyak kacang soya epoksi

REFERENCES

Biedermann, M., Fiselier, K., Marmiroli, G., Avanzini, G., Rutschmann, E., Pfenninger, S. & Grob, K. 2008. Migration from the gaskets of lids into oily foods: First results on polyadipates. European Food Research and Technology 226: 1399-1407.

Biedermann-Brem, S., Biedermann, M., Fankhauser-Noti, A., Grob, K. & Helling, R. 2007. Determination of epoxidized soy bean oil (ESBO) in oily foods by GC-FID or GC-MS analysis of the methyl diepoxy linoleate. European Food Research and Technology 224: 309-314.

Castle, L., Sharman, M. & Gilbert, J. 1988a. Analysis of the epoxidised soya bean oil additive in plastics by gas chromatography. Journal of Chromatography A 437: 274- 280.

Castle, L., Sharman, M. & Gilbert, J. 1988b. Gas chromatographic-mass spectometric determination of epoxidized soybean oil contamination of foods by migration from plastic packaging. J. Assoc. Off. Anal. Chem. 71: 1183-1186.

Ezerskis, Z., Morkunas, V., Suman, M. & Simoneau, C. 2007. Analytical screening of polyadipates and other plasticisers in poly(vinyl chloride) gasket seals and in fatty food by gas chromatography-mass spectrometry. Analytica Chimica Acta 604: 29-38.

Fankhauser-Noti, A. & Grob, K. 2006. Migration of plasticizers from PVC gaskets of lids for glass jars into oily foods: Amount of gasket material in food contact, proportion of plasticizers migrating into food and compliance testing by simulation. Trends in Food Science & Technology 17: 105-112.

Fankhauser-Noti, A., Fiselier, K., Biedermann-Brem, S. & Grob, K. 2005. Epoxidized soy bean oil migrating from the gaskets of lids into food packed in glass jars: Analysis by on-line liquid chromatography-gas chromatography. Journal of Chromatography A 1082: 214-219.

Fankhauser-Noti, A., Biedermann-Brem, S. & Grob, K. 2006. PVC plasticizers/additives migrating from the gaskets of metal closures into oily food: Swiss market survey June 2005. European Food Research and Technology 223: 447-453.

Grob, K. & Schilling, B. 1985. Coupled HPLC-Capillary GC - State of the art and outlook. Journal of High Resolution Chromatography & Chromatography Communications 8: 726-733.

Grob, K. 2000. Efficiency through combining high-performance liquid chromatography and high resolution gas chromatography: Progress 1995-1999. Journal of Chromatography A892: 407-420.

Han, L-M.T. & Szajer, G. 1994. Analysis of epoxidized soybean oil by gas chromatography. Journal of the American Oil Chemists’ Society 71: 669-670.

RASFF, Rapid Alert System For Food And Feed. http:// ec.europa.eu/food/food/rapidalert/reports/week22-2005_ en.pdf, 2005. 2005/22.

RASFF. Rapid Alert System for Food and Feed. http://ec.europa. eu/food/food/rapidalert/reports/week40-2007_en.pdf, 2007. 2007/40.

Sanagi, M.M., Ling, S.L., Nasir, Z., Hermawan, D., Ibrahim, W.A.W. & Naim, A.A. 2009. Comparison of signal-to-noise, blank determination, and linear regression methods for the estimation of detection and quantification limits for volatile organic compounds by gas chromatography. Journal of AOAC International 92(6): 1833-1838.

Suman, M., Tegola, S.L., Catellani, D. & Bersellini, U. 2005. Liquid chromatography-electrospray ionization-tandem mass spectrometry method for the determination of epoxidized soybean oil in food products. Journal of Agricultural and Food Chemistry 53: 9879-9884.

Weitzel, M.L.J., Lee, S.M., Smoot, M., Viafara, N. & Brodsky, M. 2007. The Analytical Laboratory Accreditation Criteria Committee (ALACC) Guide: How to Meet ISO 17025 Requirements for Method Verification. Gaithersburg, Maryland, USA: AOAC International.

*Corresponding author; email: marsin@kimia.fs.utm.my