Abstract
A simple, fast and ecological analytical method using a semi-automatic fat extractor and HPLC-FLD (fluorescence detection) for determination of polycyclic aromatic hydrocarbon markers i.e. benzo(a)anthracene (BaA), chrysene (Chr), benzo(a)pyrene (BaP) and benzo(b)fluoranthene (BbF) in cocoa butter has been validated. Validation’s procedure performed out in concordance with French standard NF V03-110 (2010) was based on existing polycyclic aromatic hydrocarbon (PAH) determination methods in various smoked foodstuffs and edible vegetable oils. Determination of correlation coefficients for specific PAHs ranged from 0.9992 to 0.9998. Respective values of limits of detection were 0.010, 0.011, 0.033 and 0.029 μg kg−1 and those of quantification were 0.035, 0.038, 0.111 and 0.098 μg kg−1 for BaA, Chr, BbF and BaP. Both values of repeatability and intermediary precision tests coefficients of variation were less than 5%. Recovery scores of four PAH markers matched EU standard 836/2011 recommendations. Sum of four PAH markers (BaA, Chr, BbF, BaP) contents varied from 5.42 ± 0.58 to 11.37 ± 0.01 μg kg−1 whereas those of BaP was comprised between 0.26 ± 0.00 and 1.75 ± 0.13 μg kg−1 in 20 cocoa butter samples extracted from raw cocoa bean stored at Ivorian cocoa farmer levels.
Similar content being viewed by others
References
Beckett ST, Fowler MS, Ziegler GR (2017) Beckett’s industrial chocolate manufacture and use, 5th edn. Wiley-Blackwell, Oxford
Bratinova S, Karasek L, Buttinger G, Wenzl T (2015) Report on the 16th inter-laboratory comparison organized by the European Union reference laboratory for polycyclic aromatic hydrocarbons. EUR 27558:15. https://doi.org/10.2787/279750
Dost K, Ideli C (2012) Determination of polycyclic aromatic hydrocarbons in edible oils and barbecued food by HPLC/UV–Vis detection. Food Chem 133:193–199
EFSA (2008) Scientific opinion of the panel on contaminants in the food chain on a request from the European commission on polycyclic aromatic hydrocarbons in food. EFSA J 724:1–114
European Commission (2011) Commission regulation (EU) N° 835/2011 of 19 August 2011 amending regulation (EC) no 1881/2006 as regards maximum levels for polycyclic aromatic hydrocarbons in foodstuffs. Off J Eur Union L215:4
European Commission (2015) Commission regulation (EU) N° 2015/1933 of 27 October 2015 amending regulation (EC) no 1881/2006 as regards maximum levels for polycyclic aromatic hydrocarbons in cocoa fiber, banana chips, food supplements, dried herbs and dried spices. Off J Eur Union L 282/11, 3
FAO (1997) Validation of analytical methods for food control—Vienna. Report of Joint FAO/IAEA Expert Consultation, p. 18
Farhadian A, Jinap S, Abas F, Sakar ZI (2010) Determination of polycyclic aromatic hydrocarbons in grilled meat. Food Control 21:606–610
Guehi TS, Bi Zahouli I, Ban-Koffi L, Monke AF, Nemlin JG (2010) Performance of different drying methods and their effects on the chemical quality attributes of raw cocoa material. Int J Food Sci Technol 45:1564–1571
Guehi TS, Dingkuhn M, Cros E, Fourny G, Ratomahenina R, Moulin G, Vidal AC (2008a) Impact of cocoa processing technologies in free fatty acids formation in stored raw cocoa beans. Afr J Agric Res 3(3):174–179
Guehi TS, Yao ND, Manizan NP, Nevry KR, Koffi BL, Konan YM (2008b) Comparison of the degree of fermentation and fungal profiles of raw cocoa beans sourced from three Ivorian main producing regions. Afr J Agric Res 2:112–118
Houessou JK, Delteil C, Camel V (2006) Investigation of sample treatment steps for the analysis of polycyclic aromatic hydrocarbons in ground coffee. J Agric Food Chem 54(20):7413–7421
ICCO (2017) Quarterly bulletin of cocoa statistics, Vol. XLIII, No. 1, Cocoa year 2016/17, Consulted 28-02-2017
Ishizaki A, Saito K, Hanioka N, Narimatsu S, Kataoka H (2010) Determination of polycyclic aromatic hydrocarbons in food samples by automated on-line in-tube solid-phase microextraction coupled with high-performance liquid chromatography-fluorescence detection. J Chromatogr A 1217:5555–5563
ISO (2016–04) Animals and vegetables fats and oils—determination of polycyclic aromatic Hydrocarbons. ISO 15753:2016: International Organization for Standardization
ISO (1980-12-01). Cocoa beans—determination of moisture content (routine method) ISO 2291:1980: International Organization for Standardization
Jira W, Ziegenhals K, Speer K (2008) Gas chromatography mass spectrometry (GC-MS) method for the determination of 16 European priority polycyclic aromatic hydrocarbons in smoked meat products and edible oils. Food Addit Contam 25:704–713
Lee BM, Shim GA (2007) Dietary exposure estimation of benzo[a]pyrene and cancer risk assessment. J Toxicol Environ Health Part A 70:1391–1394
Lee ML, Novotny M, Bartle KD (1981) Analytical chemistry of polycyclic aromatic compounds. Academic Press, New York, pp 98–102
Lin D, Tu Y, Zhu L (2005) Concentrations and health risk of polycyclic aromatic hydrocarbons. Food Chem Toxicol 43(1):41–48
NF V03-110 (2010) Analyse des produits agricoles et alimentaires : Procédure de validation intra-laboratoire d’une méthode alternative par rapport à une méthode de référence. Paris Edition AFNOR, p. 40
Raters M, Matissek R (2014) Quantitation of polycyclic aromatic hydrocarbons (PAH4) in cocoa and chocolate samples by an HPLC-FD method. J Agric Foods Chem 62:10666–10671
Rodríguez-Acuña R, Pérez-Camino MC, Cert A, Moreda W (2008) Sources of contamination by polycyclic aromatic hydrocarbons in Spanish virgin olive oils. Food Addit Contam Part A 25(1):115–122
Rozentāle I, Stumpe-Vīksna I, Začs D, Siksna I, Melngaile A, Bartkevičs V (2015) Assessment of dietary exposure to polycyclic aromatic hydrocarbons from smoked meat products produced in Latvia. Food Control 54:16–22
Servent A, Boulanger R, Davrieux F, Pinot M-N, Tardan E, Forestier-Chiron N, Hue C (2017) Assessment of cocoa (Theobroma cacao L.) butter content and composition throughout fermentations. doi:https://doi.org/10.1016/j.foodres.2018.02.070
Simko P (2002) Determination of polycyclic aromatic hydrocarbons in smoked meat products and smoke flavouring food additives. J Chromatogr B Analyt Technol Biomed Life Sci 770(1–2):3–18
Simon R, Gomez Ruiz JA, Von Holst C, Wenzl T, Anklam E (2008) Results of a European inter-laboratory comparison study on the determination of EU priority polycyclic aromatic hydrocarbons (PAHs) in edible vegetable oils. Anal Bioanal Chem 391(4):1397–1408
Wenzl T, Simon R, Anklam E, Kleiner J (2006) Analytical methods for polycyclic aromatic hydrocarbons (PAHs) in food and the environment needed for new food legislation in the European Union. Trends Anal Chem 25:716–725
Whitefield R (2005) Making chocolates in the factory. Kennedy’s Publications Ltd., London
Zachara A, Galkowska D, Juszczak L (2017) Method validation and determination of polycyclic aromatic hydrocarbons in vegetable oils by HPLC-FLD. Food Anal Methods 10:1078–1086. https://doi.org/10.1007/s12161-016-0673-5
Zelinkova Z, Wenzl T (2015) EU marker polycyclic aromatic hydrocarbons in food supplements: analytical approach and occurrence. Food Addit Contam Part A 32(11):1914–1926
Zougagh M, Redigolo H, Rios A, Valcarcel M (2004) Screening and confirmation of PAHs in vegetable oil samples by use of supercritical fluid extraction in conjunction with liquid chromatography and fluorimetric detection. Anal Chim Acta 525:265–271
Zyzelewicz D, Oracz J, Krysiak W, Budryn G, Nebesny E (2017) Effects of various roasting conditions on acrylamide, acrolein and polycyclic aromatic hydrocarbons content in cocoa bean and the derived chocolates. Dry Technol 35(3):363–374
Acknowledgements
This work was supported by the Food Safety Team of UMR Qualisud of Cirad, Montpellier, France, and by the Research Group on Post-Harvest Technology and Quality of Cocoa of Food Sciences and Technology Department (UFR-STA) of University Nangui ABROGOUA, Abidjan, Côte d’Ivoire.
Funding
This research was funded by a grant for Ivorian PhD students No. 2014/BE_033D/C2D_AMRUGE-CI awarded by AMRUGE/C2D COTE D’IVOIRE.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of Interest
Didier-Axel Sees-Tchotch has received research grants from AMRUGE/C2D COTE D’IVOIRE. Didier-Axel Sess-Tchotch declares that he has no conflict of interest. Kra Brou Didier Kedjebo declares that he has no conflict of interest. Betty Meuwiah Faulet declares that she has no conflict of interest. Angelique Fontana-Tachon declares that she has no conflict of interest. Pascaline Alter declares that she has no conflict of interest. Noël Durand declares that he has no conflict of interest. Joël Grabulos declares that he has no conflict of interest. Didier Montet declares that he has no conflict of interest. Tagro Simplice Guehi declares that he has no conflict of interest.
Ethical Approval
This article does not contain any studies with human participants or animals performed by any of the authors.
Informed Consent
All co-authors have given their consent for publication of this paper in the Food Analytical Method journal.
Rights and permissions
About this article
Cite this article
Sess-Tchotch, DA., Kedjebo, K.B.D., Faulet, B.M. et al. Analytical Method Validation and Rapid Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Cocoa Butter Using HPLC-FLD. Food Anal. Methods 11, 3138–3146 (2018). https://doi.org/10.1007/s12161-018-1282-2
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-018-1282-2