1. 中国计量科学研究院分析科学与化学计量研究所
2. 中国医学科学研究院药物研究所
3. 江苏省计量科学研究院化学所
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马康, 杨亚楠, 邢金京, 等. 诱惑红溶液标准物质的研制及不确定度评定[J]. 分析测试学报, 2012,31(3):296-301.
Preparation and Certification of A Certified Reference Material Allure Red Solution and Its Uncertainty Evaluation[J]. 2012,31(3):296-301.
建立了食用合成色素诱惑红溶液标准物质的制备和定值方法,研制了100 mg/L的诱惑红溶液标准物质。采用制备液相色谱对筛选的市售原料纯化,得到纯度大于99%的诱惑红纯品;通过核磁共振(1H NMR谱)和液相色谱-质谱(HPLC-LTQ/MS)准确定性分析后,利用高效液相色谱法(HPLC)对诱惑红纯物质进行纯度定值。以0.1 mol/L乙酸铵和甲醇为流动相进行等度洗脱,采用Intersil ODS-C18(250 mm×4.6 mm,5 μm)进行分离,检测波长240 nm。为保证纯度测量的准确性,采用多家联合定值对诱惑红的纯度进行定值,诱惑红纯物质的定值纯度为99.61%(λ=240 nm)。诱惑红溶液标准物质经重量-容量法配制后,进行均匀性和稳定性实验,浓度赋值后进行不确定度评定,诱惑红溶液的量值为100 mg/L,扩展相对不确定度为1.0%(k=2)。该溶液标准物质已批准为国家级标准物质,可为相关部门提供检测标准。
A methodology regarding the preparation and certification of certified reference material (CRM) of allure red solution was presented.After the qualitative analysis on pure substance of allure red by liquid chromatography-mass spectrometry(LC-LTQ/MS) and 1H NMR spectrum,the purity of allure red was certified by high performance liquid chromatography(HPLC),the purity certification of allure red was performed at 240 nm with methanol and 0.1 mol/L ammonium acetate solution as mobile phase,and the Intersil ODS-C18 column(250 mm×4.6 mm,5 μm) was used for analysis.The certification purity of allure red was 99.61%.To verify the result,six certification labs were performed,at the same time,the water content and volatile impurity were determined by the total gravimetric analysis(TGA).Allure red solution CRM was prepared by the gravity-volume method.After the tests of homogeneity and stability,the concentration of allure red solution CRM was certified and the uncertainty was evaluated.The certified result was 100 mg/L and the expanded relative uncertainty was 1.0%(k=2).The allure red solution CRM was approved as a national CRM and could be applied in food safety detection.
诱惑红溶液标准物质液相色谱法不确定度评定
allure redsolution certified reference materialhigh performance liquid chromatographyuncertainty evaluation
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