CCQM-K95.1 Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea

David L Duewer ,Jacolin A Murray ,Laura J Wood ,Stephen A Wise ,Sebastian Hein ,Matthias Koch ,Rosemarie Philipp ,Martina Werneburg ,Rudolf Hackenberg ,Joachim Polzer ,M Avila ,Victor Serrano ,Elias Kakoulides ,Charalampos Alexopoulos ,Panagiota Giannikopoulou ,Ee Mei Gui ,Ting Lu ,Tang Lin Teo ,Tang Hua ,Chen Dazhou ,Li Chunxin ,Ye Changjun ,Li Hongmei ,Jintana Nammoonnoy ,Lane C Sander ,Katrice A Lippa ,Laura Quinn ,C Swiegelaar ,Maria Fernandes-Whaley ,Ahmet C Gören ,Taner Gokcen

doi:10.1002/https://doi.org/10.1088/0026-1394/56/1a/08002

Abstract

Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography.

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