بهینه سازی شرایط استخراج ملامین و تعیین میزان آن در تخم مرغ به روش کروماتوگرافی مایع با کارایی بالا

نویسندگان
مسعود حاجی سلیمانی 1
شعله عطایی 1
علی گنجلو 2
1 مرکز خدمات تخصصی کنترل کیفی و کمی آب و مواد غذایی جهاد دانشگاهی واحد زنجان، ایران
2 گروه علوم و مهندسی صنایع غذایی- دانشکده کشاورزی- دانشگاه زنجان
چکیده
وجود ملامین در مواد غذایی یکی از موضوعات حائز اهمیت در زمینه ایمنی مواد غذایی و سلامت مصرف کنندگان می­باشد. استخراج اولین قدم در راستای تعیین میزان ملامین در مواد غذایی است. لذا در پژوهش حاضر شرایط استخراج ملامین از تخم مرغ با استفاده از روش شناسی سطح پاسخ بر اساس طرح مرکب مرکزی بهینه گردید. درصد آب در فاز استخراج کننده حاوی آب/استونیتریل، حجم فاز استخراج کننده، زمان استخراج، pH فاز استخراج کننده و غلظت هیدروکلریک اسید در فاز استخراج کننده به عنوان متغیرهای مورد مطالعه برای بهینه سازی استخراج ملامین در نظر گرفته شدند. در نهایت مقدار ملامین موجود در چهار نشان تجاری تخم مرغ با استفاده از دستگاه کروماتوگرافی مایع با کارآیی بالا (HPLC) به­ روش افزایش استاندارد اندازه‌گیری شد. شرایط بهینه استخراج به صورت 28/39 درصد آب در فاز استخراج کننده، 06/5 میلی­لیتر حجم حلال استخراج کننده، 48/12 دقیقه زمان استخراج، pH برابر 04/5 و غلظت اسید برابر 73/0 مولار به دست آمد. مقدار ملامین در نمونه‌های تخم مرغ مورد مطالعه در محدوده 45/0-19/0 میلی‌گرم بر کیلوگرم به دست آمد. با توجه به میزان مجاز ملامین که توسط اتحادیه اروپا و سازمان غذا و داروی آمریکا تعیین شده است می­توان نتیجه گیری نمود که مقدار ملامین نمونه­­های مورد مطالعه در محدوده مجاز استاندارد اتحادیه اروپا قرار دارد و تنها در دو نمونه مقدار آن بیش از استاندارد آمریکا است.
کلیدواژه‌ها
بهینه سازی
استخراج
ملامین
تخم مرغ
کروماتوگرافی مایع با کارآیی بالا

موضوعات

عنوان مقاله English

Optimization of extraction conditions and determination of melamine in egg using high-performance liquid chromatography

نویسندگان English

Masoud Haji Soliemani 1
Sholeh Attaye 1
Ali Ganjloo 2
1 Quantitative and Qualitative Food and Water Control Center of Jahad Daneshgahi, Zanjan Branch, Zanjan, Iran
2 Department of Food Science and Engineering-Faculty of Agriculture-University of Zanjan
چکیده English

The presence of melamine in foods is one of the important issues in terms of food safety and consumer health. Extraction is the first step in determining the amount of melamine in foods. Therefore, in the current study, melamine extraction from egg was optimized using response surface methodology based on the central composite design. The percentage of water used in the extraction phase containing water/acetonitrile, extraction phase volume, extraction time, pH of extraction phase, and hydrochloric acid concentration in the extraction phase were considered as the studied variables for optimizing extraction conditions. Finally, the amount of melamine present in four brands of egg was measured by high-performance liquid chromatography (HPLC) using internal standard method. Optimum extraction conditions were obtained in the form of 39.28% water in the extraction phase, 5.06 mL extraction solvent volume, 12.48 min extraction time, pH 5.04 and acid concentration of 0.73 M. The amount of melamine in the egg samples was in the range of 0.19-0.45 mg/kg. Regarding the amount of melamine authorized by the EU and the US Food and Drug Administration, it can be concluded that the melamine content of the samples is within the limits of the EU standard and only in two samples was more of the USFDA standard.

کلیدواژه‌ها English

Optimization
Extraction
Melamine
Egg
High-Performance Liquid Chromatography
[1] OECD. 1998. Screening Information Data Set for Melamine, CAS No. #108-78-1 read at http://www.chem.unep.ch/irptc/sids/OECDSIDS/108781.pdf, 17 Sept 2008.
[2] Chen, Z., Yan, X. 2009. Simultaneous determination of melamine and 5-hydroxymethylfurfural in milk by capillary electrophoresiswith diode array detection. Journal of Agricultural and Food Chemistry, 57, 8742-8747.
[3] Tyan, Y.C., Yang, M.H., Jong, S.B., Wang, C.K., Shiea, J. 2009. Melamine contamination. Analytical and Bioanalytical Chemistry, 395, 729-735.
[4] Sancho, J.V., Ibanez, M., Grimalt, S., Pozo, O.J., Hernandez, F. 2005. Residue determination of cyromazine and its metabolite melamine in chard samples by ion-pair liquid chromatography coupled to electrospray tandem mass spectrometry. Analytica Chimica Acta, 530, 237-243.
[5] El-Sayed, W.S,. El-Bazو A.F., Othman, A.M. 2006. Biodegradation of melamine formaldehyde by Micrococcus sp.strain MF-1 isolated from aminoplastic waste water effluent. International Biodeterioration and Biodegradation, 57, 75-81.
[6] Brown, C.A., Jeong, K.S., Poppenga, R.H., Puschner, B., Miller, D.M., Ellis, A.E. 2007. Outbreaks of renal failure associated with melamine and cyanuric acid in dogs and cats in 2004 and 2007. Journal of Veterinary Diagnostic Investigation,19, 525-531.
[7] Bizzari, S., Yokose, K. 2008. Melamine. In: Chemical economics handbook. Menlo Park, CA, SRI ConsultingInc.(http://www.sriconsulting.com/CEH/Public/Reports/673.3000/).
[8] Baldree, L.A., Stapleton, F.B. 1990. Uric acid metabolism in children. Pediatric Clinics of North America, 37, 391-418.
[9] Xu, X.M., Ren, Y.P., Zhu, Y., Cai, Z.X., Han, J.I., Huang, B.F. 2009. Direct determination of melamine in dairy productsby gas chromatography/mass spectrometry with coupled column separation. Analytica Chimica Acta, 650, 39-43.
[10] Gossner, C.M.E., Schlundt, J., Embarek, P.B., Hird, S., Wong, D., Lo-Fo-., Beltran, J.J.O. 2009. The melamine incident: Implications for international food and feed safety. Environmental Health Perspectives,117, 1803-1808.
[11] Dobson, R.L., Motlagh, S., Quijano, M., Cambron, R.T., Baker, T.R., Pullen, A.M. 2008. Identification and characterization of toxicity of contaminants in pet food leading to an outbreak of renal toxicity in cats and dogs. Toxicilogical Sciences, 106(1), 251-262.
[12] Guo, Z., Gai, P., Hao, T., Wang, S., Wei, D., Gan, N. 2011. Determination of melamine in dairy products by an electrochemiluminescent method combined with solid-phase extraction. Talanta, 83, 1736-1741.
[13] Wu, Q.Q., Fan, K.X., Sha, W., Ruan, H.Q., Zeng, R., Shieh, C.H. 2009. Highly sensitive detection of melamine based on reversed phase liquid chromatography mass spectrometry. Chinese Science Bulletin, 54, 732-737.
[14] Ehling, S., Tefera, S., Ho, I.P. 2007. High-performance liquid chromatographic method for the simultaneous detection of the adulteration of cereal flours with melamine and related triazine by-products ammeline, ammelide, andcyanuric acid. Food Additives and Contaminants, 24, 1319-1325.
[15] Venkatasami, G., Sowa, J.R. 2010. A rapid, acetonitrile-free, HPLC method for determination of melamine in infant formula. Analytica Chimica Acta, 665, 227- 230.
[16] Sun, F.X., Ma, W., Xu, L.G., Zhu, Y.Y., Liu, L.Q., Peng, C.F. 2010. Analytical methods and recent developments in the detection of melamine. Journal of Zhejiang university Science B, 29, 1239-1294.
[17] Tian, Y., Chen, L., Gao, L., Wu, M., Dick, W.A. 2012. Comparison of three methods for detection of melamine in compost and soil. Science of the Total Environment, 417-418, 255-262.
[18] Tittlemier, S.A., Lau, B.P.Y., Menard, C., Corrigan, C., Sparling, M., Gaertner, D. 2009. Melamine in infant formula sold in Canada: Occurrence and risk assessment. Journal of Agricultural and Food Chemistry, 57, 5340-5344.
[19] Zheng, X.L., Sheng, B.Y., Xian, K.L., Dai, Y.N. 2012. Determination of melamine in dairy products by HPLC-UV with NH2 column. Food Control, 23, 245-250.
[20] Health Canada. 2008. The Government of Canada responds to reports of melamine in food products. Ottawa, Ontario, Health Canada, 3 October 2008 (http://www.hc-sc.gc.ca/fn-an/securit/chem-chim/melamine-eng.php).
[21] Wei, F., Lam, R., Cheng, S., Lu, S., Ho, D., Li, N. 2010. Rapid detection of melamine in whole milk mediated by unmodified gold nanoparticles. Applied Physsics Letters, 96(13), 133702.
[22] Sun, H.W., Wang, L.X,, Ai, L.F., Liang, S.X. 2010. A sensitive and validated method for determination of melamine residue in liquid milk by reversed phase high performance liquid chromatography with solid-phase extraction. Food Control, 21(5), 686-691.
[23] Smoker, M., Krynitsky, A.J. 2008. Interim method for determination of melamine and cyanuric acid residues in foods using LC-MS/MS: Version 1.0. U.S. Food and Drug Administration (FDA), Available from http://www.fda.gov/Food/ScienceResearch/LaboratoryMethods/DrugChemicalResiduesMethodology/ucm071673.htm.
[24] Li, J., Qia, H.Y., Shi, Y.P. 2009. Determination of melamine residues in milk products by zirconia hollow fiber sorptive micro extraction and gas chromatography-mass spectrometry. Journal of Chromatography A,1216, 5467-5471.
[25] Miao, H., Fan, S., Wu, Y.N., Zhang, L., Zhou, P.P., Li, J.G. 2009. Simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products by gas chromatography-tandem mass spectrometry. Biomedical Environmrntal Sciences, 22(2), 87-94.
[26] Bimakr, M., Rahman, R.A., Salina Taip, F., Adzahan, N.M., Sarker, M.Z.I., Ganjloo, A. 2013. Supercritical carbon dioxide extraction of seed oil from winter melon (Benincasa hispida) and its antioxidant activity and fatty acid composition. Molecules, 18, 997-1014.
[27] ArminFashi, A.,Yaftiana, M. R., Zamani, A A. (2015). Determination of melamine in dairy products using electromembrane–LPME followed by HPLC. Food Chemistry, 188, 92-98.
[28] Sarafraz Yazdi, A., Raouf Yazdinezhad, S., Heidari, T. (2015). Determination of melamine in soil samples using surfactant-enhanced hollow fiber liquid phase microextraction followed by HPLC–UV using experimental design. Journal of Advanced Research, 6(6), 957-966.
[29] Anirudhan, T.S., Christa, J., Deepa, J.R. (2017). Extraction of melamine from milk using a magnetic molecularly imprinted polymer. Food Chemistry, 227, 85-92.
[30] Hyuk Suh, J., Jung, J., Kim, B., Cho, H-D., Kim, J., Eom, T., Park, M., Wang, Y., Beom Han, S. (2017). Development of aqueous mobile phase using chaotrope for the chromatographic determination of melamine in infant formula. Journal of Chromatography A, 1496.
مجله علوم و صنایع غذایی ایران
دوره 16، شماره 88
خرداد 1398
صفحه 147-160