Ma Jiahui, Luo Shuangxia, Li Xiaomin, Zhao Xiaotong, Li Xiuqin, Zhang Qinghe, Yin Xiong
College of Chemistry, State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, P. R. China.
Food Safety Analysis Laboratory, Division of Chemical Metrology and Analytical Science, National Institute of Metrology, Beijing 100029, P. R. China.
ACS Omega. 2025 Jun 1;10(22):23601-23608. doi: 10.1021/acsomega.5c02463. eCollection 2025 Jun 10.
Well-characterized solution certified reference materials (CRMs) are necessary for the accurate determination, quality control, instrument calibration, and validation of analytical approach. Simultaneously, a mixed solution CRM of vanillin spices is in high demand because of the accurate measurement and traceability of vanillin spices in various food matrices. In this study, a mixed vanillin spices acetonitrile CRM (issued with GBWE 086557), including methylvanillin, ethylvanillin, vanillin, and coumarin, has been developed using the gravimetric method by the National Institute of Metrology, China. Methylvanillin, ethylvanillin, and vanillin showed poor stability in methanol. The acetalization of the aldehyde group of vanillin was the major step during the degradation process, as elucidated by ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS), and exposure to high temperature and light irradiation accelerated the degradation dramatically, whereas the acetonitrile CRMs held sufficient homogeneity, and they were stored stable at 4 °C over 9 months or 50 °C for 7 days. Typically, the certified values for methylvanillin, ethylvanillin, vanillin, and coumarin in CRM were 10.1 ± 0.2, 10.2 ± 0.2, 10.0 ± 0.3, and 10.0 ± 0.2 μg/mL ( 2), respectively.
特性良好的溶液标准物质（CRMs）对于准确测定、质量控制、仪器校准以及分析方法验证而言必不可少。同时，由于香草香料在各种食品基质中的准确测量和可追溯性，香草香料混合溶液CRM的需求很高。在本研究中，中国计量科学研究院采用重量法研制了一种香草香料乙腈混合CRM（编号为GBWE 086557），其中包括甲基香草醛、乙基香草醛、香草醛和香豆素。甲基香草醛、乙基香草醛和香草醛在甲醇中稳定性较差。超高效液相色谱串联质谱（UPLC-MS/MS）表明，香草醛醛基的缩醛化是降解过程中的主要步骤，高温和光照会显著加速降解，而乙腈CRMs具有足够的均匀性，在4℃下可稳定保存9个月或在50℃下保存7天。通常，CRM中甲基香草醛、乙基香草醛、香草醛和香豆素的标准值分别为10.1±0.2、10.2±0.2、10.0±0.3和10.0±0.2μg/mL（2）。
