Determination of Lead and Cadmium Elements in Milk Chocolate with ICP-OES and Method Validation Study

Yıl 2022, Cilt: 5 Sayı: 2, 871 - 884, 18.07.2022

Fatma Hepsağ , İbrahim Hayoğlu

https://doi.org/10.47495/okufbed.1040272

Öz

In this study, a method validation study was performed for the determination of lead (Pb), cadmium (Cd) elements in chocolate by inductively coupled plasma optical emission spectrometry (ICP-OES). As the validation parameters, determination limit (LOD), measurement limit (LOQ), linear measurement range, sensitivity and precision were determined. Certified Reference Materials (CRM) were used in the study. Repeatability was in the range of 0,0365-1,197 ppm for Pb, 0,064-0,247 ppm for Cd, accuracy between 0,365-1,255 and 0,065-0,247 ppm, respectively. Recovery rates were determined as 71,51-96,56% and 64,10-88,05%. In the study, 20 milk chocolate samples were examined, Pb and Cd concentrations were determined between 0,004-0,009 and 0,001-0,002 ppm, respectively, and LOD and LOQ values were calculated as 0,005 and 0,016 for Pb, 0,001 and 0,002 for Cd. The results obtained, Eurachem “The Fitness for Purpose of Analytical Methods” Second Edition 2014 and NMKL 161 method and Turkish Food Codex “Lead, cadmium, mercury, inorganic tin, 3-MCPD, 2 diol and polycyclic aromatic hydrocarbon levels in foods sampling, sample preparation and analysis method criteria were found to be appropriate for the control according to the communique (Communique No: 2014/2).

Anahtar Kelimeler

Chocolate, Cadmium, Lead, Cocoa, Validation, ICP-OES

Sütlü Çikolatalarda Kurşun ve Kadmiyum Elementlerinin ICP-OES ile Tespiti ve Metod Validasyon Çalışması

Öz

Bu çalışmada, indüktif olarak eşleşmiş plazma optik emisyon spektrometresi (ICP-OES) ile çikolatada kurşun (Pb), kadmiyum (Cd) elementlerin tespiti için metod validasyon çalışması yapılmıştır. Validasyon parametreleri olarak, tayin limiti (LOD), ölçüm limiti (LOQ), lineer ölçüm aralığı, hassasiyet ve kesinlik belirlenmiştir. Çalışmada, Sertifikalı Referans Materyalleri (CRM) kullanılmıştır. Tekrarlanabilirlik, Pb için 0.0365-1.197 ppm, Cd için 0.064-0.247 ppm, doğruluk sırasıyla 0.365-1.255 ve 0.065-0.247 ppm aralığında idi. Geri kazanım oranları ise %71.51-96.56 ve %64.10-88.05 olarak belirlenmiştir. Çalışmada 20 sütlü çikolata örnekleri incelenmiş olup, Pb ve Cd konsantrasyonları sırasıyla 0.004-0.009 ve 0.001-0.002 ppm aralığında tespit edilmiş olup LOD ve LOQ değerleri Pb için 0.005 ve 0.016, Cd için 0.001 ve 0.002 olarak hesaplanmıştır. Elde edilen sonuçların, Eurachem “ The fitness for purpose of Analytical Methods” Second Edition 2014’e ve NMKL 161 metodu ve Türk Gıda Kodeksi “Gıdalarda kurşun, kadmiyum, cıva, inorganik kalay, 3-MCPD, 2 diol ve polisiklik aromatik hidrokarbon seviyelerinin resmi kontrolü için numune alma, numune hazırlama ve analiz metodu kriterleri tebliğine (Tebliğ No: 2014/2) göre uygun olduğu görülmüştür.

Anahtar Kelimeler

Çikolata, kadmiyum, kurşun, kakao, validasyon

Kaynakça

• Abt, E., Sam, J.F., Gray, P., Robin, L.P. Cadmium and leas in cocoa powder and chocolate products in the US Market. Food Additives & Contaminants: Part B 2018; 11(2): 92-102.
• Bruinsma, K., Taren, D.L. Chocolate: food or drug. Journal of The American Dietetic Association, 1999; 99: 1249-1256.
• Chavez, E., He, Z.L., Stoffella, P.J., Mylavarapu, R., Li, Y., Baligar, V.C. Evaluation of soil amendments as a remediation alternative for cadmium-contaminated soils under cacao plantations. Environmental Science Pollution Research 2016a; 23: 17571–17580.
• Chavez, E., He, Z.L., Stoffella, P.J., Mylavarapu, R.S., Li, Y.C., Baligar, V.C. Chemical speciation of cadmium: an approach to evaluate plant-available cadmium in Ecuadorian soils under cacao production. Chemosphere 2016b; 150: 57–62.
• Crozier, S.J., Preston, A.G., Hurst, J.W., Payne, M.J., Mann, J., Hainly, L., Miller, D.L. Cacao seeds are a “super fruit”: A comparative analysis of various fruit powders and products. Chemistry Central Journal 2001; 5: 1-6.
• Dahiya, S., Karpe, R., Hedge, A.G., Sharma, R.M. Lead, cadmium and nickel in chocolates and candies from suburban areas of Mumbai, India. Journal Food Composition and Analysis 2005; 18: 517-522.
• Duran, A., Tuzen, M., Soyla, M. Trace metal contents in chewing gums and candies marketed in Turkey. Environmental Monitoring and Assessment 2009; 149: 283–289.
• EFSA. Cadmium dietary exposure in the European population EFSA Journal 2012; 10 (1).
• EURACHEM GUIDE. The Fitness for Purpose of Analytical Methods-A Laboratory Guide to Method Validation and Related Topics 2014; Second Edition.
• Figurska-Ciura, D., Styczynska, M., Malicki, A., Bruzewicz, S. Zawartosc wybranych matali ciezkich oraz zanieczyszczen mikrobiologicznych wyrobach czekoladowych. Acta Scientiarum Polonorum Medicina Veterinaria 2006; 5: 57-63.
• Gramlich, A., Tandy, S., Gauggel, C., Lopez, M., Peria, D.G., Schulin, R. Soil cadmium uptake by cocoa in Honduras. 18th International Conference on Heavy Metals in the Environment, Ghent, 2016; Belgium.
• Gramlich, A., Tandy, S., Andres, C., Paniagua, J.C., Armengot, L., Schneider, M., Schulin, R. Cadmium uptake by cocoa trees in agroforestry and monoculture systems under conventional and organic management. The Science of the Total Environment 2017; 580: 677–686.
• Grivetti, L.I., Shapiro, H. Chocolate: History, Culture and Heritage, Wiley, 2009; Hoboken.
• IARC. Traditional herbal medicines, some mycotoxins, naphthalene and styrene, IARC Monographs on the evaluation of carcinogenic risks to humans, Lyon, France: International Agency for Research on Cancer 2002; 82: 1–556.
• IARC. Monographs on the evaluation of carcinogenic risks to humans: chemical agents and related occupations, A review of human carcinogens, Lyon, France: International Agency for Research on Cancer 2012; 100: 224–248.
• Kruszewski, B., Obiedziński,, M.W., Kowalska, J. Nickel, cadmium and lead levels in raw cocoa and processed chocolate mass materials from three different manufacturers. Journal of Food Composition and Analysis 2018; 66: 127–135.
• Lee, C.K., Low, K.S. Determination of cadmium, lead, copper and arsenic in raw cocoa, semi finished and finished chocolate products. Pertanika 1985; 8: 243-248.
• Manton, W.I.I.M. Determination of the provenance of cocoa by soil protolith ages and assessment of anthropogenic lead Contamination by Pb/Nd and lead isotope ratios. Journal of Agricultural and Food Chemistry 2010; 58: 713-721.
• Mesallam, A.S. Heavy metal content of canned orange juice as determined by direct current plasma atomic emission spectrophotometry (DCPAES). Food Chemistry 1987; 26(1): 47-58.
• Mounicou, S., Szpunar, J., Andrey, D., Blake, C., Lobinski, R. Concentrations and bioavailability of cadmium and lead in cocoa powder and related products. Food Addition Contamination 2003; 20: 343–352.
• NMKL 161 Metodu ve Türk Gıda Kodeksi. “Gıdalarda kurşun, kadmiyum, cıva, inorganik kalay, 3-MCPD, 2 diol ve polisiklik aromatik hidrokarbon seviyelerinin resmi kontrolü için numune alma, numune hazırlama ve analiz metodu kriterleri tebliği (Tebliğ No: 2014/2) 2014. Parker, G., Parker, I., Brotchie, H. Mood state effects of chocolate. Journal of Affective Disorders 2006; 92: 149-159.
• Rankin, C.W., Nriagu, J.O., Aggarwal, J.K., Arowolo, T.A., Adebayo, K., Flegal, A.R. Lead Contamination in Cocoa and Cocoa Products: Isotopic Evidence of Global Contamination. Environmental Health Perspectives 2005; 113(10): 1344-1348.
• Rehman, S., Husnain, S.M. Assessment of trace metal contents in chocolate samples by atomic absorption spectrometry. Journal Trace Element Analysis 2012; 1: 1-11.
• Sager, M. Chocolate and cocoa products as a source of essential elements in nutrition. Journal Nutritional & Food Science 2012; 2: 1-10.
• Seifert, M., Jaritz, M., Holzinger, S., Seeber, O., Anke, M. Alimentary strontium intake: first results in Germany. Trace Elements in Medicine 2000; 17: 115-118.
• Vanderschueren, R., Montalvo, D., De Ketelaere, B., Delcour, J.A., Smolders, E. The elemental composition of chocolates is related to cacao content and origin: A multi-element fingerprinting analysis of single origin chocolates. Journal of Food Composition and Analysis 2019; 83: 103277.
• Villa, J.E.L., Peixoto, R.R.A., Cadore, S. Cadmium and lead in chocolates commercialized in Brazil. Journal Agriculture and Food Chemistry 2014; 62: 8759-8763.
• Yanus, R.L., Sela, H., Borojovich, E.J.C., Zakon, Y., Saphier, M., Nikolski, A., Gutflais, E., Lorber A., Karpas, Z. Trace elements in cocoa solids and chocolate: An ICPMS study. Talanta 2014; 119: 1-4.