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CCQM-K146.1 subsequent comparison low-polarity analyte in high fat food: benzo[a]pyrene in olive oil
Metrologia ( IF 2.1 ) Pub Date : 2021-07-09 , DOI: 10.1088/0026-1394/58/1a/08011
Xiaomin Li 1 , Hongmei Li 1 , Qinghe Zhang 1 , Xiaohua Lu 1 , Elias Kakoulides 2 , L Quinn 3 , M Fernandes-Whaley 3 , Milena Bucar-Miklavcic 4 , Erika Bester 4 , Bojan Butinar 4 , Taner Gokcen 5 , Mine Bilsel 5
Affiliation  

The Track A key comparison on the determination of benzo[a]pyrene in olive oil (CCQM-K146) organized by the CCQM was finished in 2020. This key comparison was related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and was the model system selected to align with the OAWG strategy for comparisons to underpin the food sector. Due to requests from the participants of this comparison, CCQM organized a supplementary comparison CCQM-K146.1 for those NMIs or DIs who did not participate in CCQM-K146 or wished to improve their results from CCQM-K146.

5 NMIs and DIs participated in CCQM-K146.1. Different extraction methods and SPE cartridges were applied in the sample pre-treatment. HPLC-FLD, GC-MS/MS and GC-TOF MS were applied for detection by the participants. Certified reference materials (CRMs) were adopted or pure materials assessed in house to guarantee traceability to SI for the calibrants.

NIM's result for CCQM-K146 was equivalent with the CCQM-K146 KCRV, thus they demonstrated acceptable performance in determining the measurand and their result for CCQM-K146.1 was used as the KCRV. The KCRV and u(KCRV) values were 8.69 μg/kg and 0.18 μg/kg, respectively. The random effects model obtained in CCQM-K146 suggests a dark uncertainty term (tau) is present, and the tau of CCQM-K146 normalized to CCQM-K146.1 measurand level is included in the estimation of degrees of equivalence (DoE) for the participants in CCQM-K146.1. This helps establish a consistent expectation of performance amongst the two studies, even when comparing to a different anchor KCRV.

One participant demonstrated their capabilities for this analysis, whereas the other three were all deviated from the KCRV. This supplementary comparison directly illustrates the capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 μg/kg to 1000 μg/kg in a high fat, low protein, low carbohydrate food matrix.

To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/.

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).



中文翻译:

CCQM-K146.1 后续比较高脂肪食品中的低极性分析物:橄榄油中的苯并[a]芘

由 CCQM 组织的关于测定橄榄油中苯并 [a] 芘 (CCQM-K146) 的 Track A 关键比较已于 2020 年完成。该关键比较与高脂肪、低蛋白质、低碳水化合物中的低极性分析物有关食品矩阵,并且是选择的模型系统以与 OAWG 战略保持一致,以进行比较以支持食品部门。由于本次比较参与者的要求,CCQM 为那些未参加 CCQM-K146 或希望改进其结果从 CCQM-K146 的 NMI 或 DI 组织了一次补充比较 CCQM-K146.1。

5 个 NMI 和 DI 参与了 CCQM-K146.1。样品前处理采用了不同的萃取方法和 SPE 小柱。参与者应用HPLC-FLD、GC-MS/MS和GC-TOF MS进行检测。采用经认证的标准物质 (CRM) 或内部评估纯材料,以保证校准物可追溯至 SI。

NIM 对 CCQM-K146 的结果与 CCQM-K146 KCRV 的结果相同,因此它们在确定被测量方面表现出可接受的性能,并且将 CCQM-K146.1 的结果用作 KCRV。KCRV 和u (KCRV) 值分别为 8.69 μg/kg 和 0.18 μg/kg。CCQM-K146 中获得的随机效应模型表明存在暗不确定性项 (tau),并且归一化到 CCQM-K146.1 被测量水平的 CCQM-K146 的 tau 包括在等价度 (DoE) 的估计中CCQM-K146.1 的参与者。这有助于在两项研究中建立一致的性能预期,即使与不同的锚定 KCRV 进行比较。

一名参与者展示了他们进行此分析的能力,而其他三名参与者都偏离了 KCRV。此补充比较直接说明了测定有机化合物质量分数的能力,分子量为 100 g/mol 至 500 g/mol,具有低极性 pKow < -2,质量分数范围为 0.1 μg/kg 至 1000 μg/ kg 在高脂肪、低蛋白质、低碳水化合物的食物基质中。

要访问本文的正文,请单击最终报告。请注意,此文本出现在 BIPM 密钥比较数据库 kcdb.bipm.org/ 的附录 B 中。

根据 CIPM 互认安排 (CIPM MRA) 的规定,最终报告已通过同行评审并由 CCQM 批准发布。

更新日期:2021-07-09
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