Institute for Reference Materials and Measurements, European Commission, Joint Research Centre, Retieseweg 111, Geel B-2440, Belgium.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Apr;26(4):466-74. doi: 10.1080/02652030802579148.
A recently published European Regulation requires that the artificial marker, glycerol triheptanoate (GTH), be added to processed animal by-product (ABPs) prohibited from entering the food chain. The objective of this new requirement is to allow full traceability and ensure that these materials are disposed of in a proper way. Here, we report the development and single-laboratory validation of an analytical method for the determination of GTH in meat and bone meal plus animal fat. The method comprises three steps: (1) extraction of GTH from the samples with petroleum ether when analysing meat and bone meal or dissolving the sample in n-hexane when analysing fat; (2) clean-up of the extract using commercially available SPE cartridges; (3) determination of GTH by GC/MS or GC with flame ionisation detection (FID). The results of the validation study demonstrated that the relative standard for intermediate precision varied between 2.5 and 8.2%, depending on GTH concentration and the detector utilised. In all cases, the relative recovery rate was above 96%. The limit of quantification was 16 mg kg(-1) (GTH/fat content of the sample) with MS as detector and 20 mg kg(-1) with FID. Moreover, the method has been successfully applied in a second laboratory, indicating its transferability. Considering the minimum GTH concentration in ABPs of 250 mg kg(-1), the method is considered suitable for the intended purpose and can be utilised by EU Member States laboratories for official control and monitoring.
最近发布的欧洲法规要求在禁止进入食物链的加工动物副产品（ABP）中添加人工标记物三庚酸甘油酯（GTH）。这一新要求的目的是实现完全可追溯性，并确保这些材料以适当的方式处理。在这里，我们报告了一种用于测定肉骨粉和动物脂肪中 GTH 的分析方法的开发和单实验室验证。该方法包括三个步骤：（1）用石油醚从肉骨粉样品中提取 GTH 或用正己烷溶解脂肪样品；（2）用市售 SPE 小柱对提取物进行净化；（3）用 GC/MS 或 GC-FID 测定 GTH。验证研究的结果表明，中间精密度的相对标准偏差在 2.5%至 8.2%之间变化，具体取决于 GTH 浓度和所用的检测器。在所有情况下，相对回收率均高于 96%。采用 MS 作为检测器，定量限为 16 mg kg(-1)（GTH/样品脂肪含量），采用 FID 为 20 mg kg(-1)。此外，该方法已成功应用于第二个实验室，表明其可转移性。考虑到 ABP 中 GTH 的最低浓度为 250 mg kg(-1)，该方法被认为适合预期目的，欧盟成员国实验室可用于官方控制和监测。
