APMP.QM-S8: determination of mass fraction of benzoic acid, methyl paraben and n-butyl paraben in soy sauce
Authors: Teo Tang Lin , Gui Ee Mei , Lu Ting , Cheow Pui Sze , Giannikopoulou Panagiota , Kakoulides Elias , Lampi Evgenia , Choi Sik-man , Yip Yiu-chung , Chan Pui-kwan , Hui Sin-kam , Wollinger Wagner , Carvalho Lucas J , Garrido Bruno C , Rego Eliane C P , Ahn Seonghee , Kim Byungjoo , Li Xiuqin , Guo Zhen , Styarini Dyah , Aristiawan Yosi , Ramadhaningtyas Dillani Putri , Aryana Nurhani , Ebarvia Benilda S , Dacuaya Aaron , Tongson Alleni , Aganda Kim Christopher , Fortune Thippaya Junvee , Tangtrirat Pradthana , Mungmeechai Thanarak , Gören Ahmet Ceyhan , Gündüz Simay , Yilmaz Hasibe 
Published: September 2017

The supplementary comparison APMP.QM-S8: determination of mass fraction of benzoic acid, methyl paraben and n-butyl paraben in soy sauce was coordinated by the Health Sciences Authority, Singapore under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM). Ten national metrology institutes (NMIs) or designated institutes (DIs) participated in the comparison. All the institutes participated in the comparison for benzoic acid, while six NMIs/DIs participated in the comparison for methyl paraben and n-butyl paraben. The comparison was designed to enable participating institutes to demonstrate their measurement capabilities in the determination of common preservatives in soy sauce, using procedure(s) that required simple sample preparation and selective detection in the mass fraction range of 50 to 1000 mg/kg. The demonstrated capabilities can be extended to include other polar food preservatives (e.g. sorbic acid, propionic acid and other alkyl benzoates) in water, aqueous-based beverages (e.g. fruit juices, tea extracts, sodas, sports drinks, etc) and aqueous-based condiments (e.g. vinegar, fish sauce, etc). Liquid--liquid extraction and/or dilution were applied, followed by instrumental analyses using LC-MS/MS, LC-MS, GC-MS (with or without derivatisation) or HPLC-DAD. Isotope dilution mass spectrometry was used for quantification, except in the case of a participating institute, where external calibration method was used for quantification of all three measurands. The assigned Supplementary Comparison Reference Values (SCRVs) were the medians of ten results for benzoic acid, six results for methyl paraben and six results for n-butyl paraben. Benzoic acid was assigned a SCRV of 154.55 mg/kg with a combined standard uncertainty of 0.94 mg/kg, methyl paraben was assigned a SCRV of 100.95 mg/kg with a combined standard uncertainty of 0.40 mg/kg, and n-butyl paraben was assigned a SCRV of 99.05 mg/kg with a combined standard uncertainty of 1.36 mg/kg. The k-factors for the estimation of the expanded uncertainties of the SCRVs were 2.26, 2.57 and 2.57, respectively. The degree of equivalence (with the SCRV) and its uncertainty were calculated for each result. All the participating institutes (except in one case for benzoic acid) were able to demonstrate or confirm their capabilities in the determination of polar food preservatives in water or aqueous-based beverages/condiments.

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The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).