三甲基吡嗪纯度标准物质的研制  

Development of the reference material for the purity of 2,3,5-trimethylpyrazine

作　　者：赵博[1] 李晓敏[1] 张庆合[1] ZHAO Bo;LI Xiao-Min;ZHANG Qing-He(National institute of metrology,Beijing 100029,China)

机构地区：[1]中国计量科学研究院,北京100029

出　　处：《食品安全质量检测学报》2018年第15期3913-3921,共9页Journal of Food Safety and Quality

基　　金：国家重大科学仪器专项(2012YQ09016703)~~

摘　　要：目的建立三甲基吡嗪纯度标准物质的定值及不确定度评定的方法。方法通过气相色谱-质谱法(gas chromatography-mass spectrometry,GC-MS)、红外光谱法(fourier transform infrared spectroscopy,FT-IR)和核磁共振法(nuclear magnetic resonance,NMR)对样品进行了定性分析。采用高效液相色谱法-二极管阵列检测器(high performance liquid chromatography-diode array detector,HPLC-DAD)和气相色谱火焰离子化检测器(gas chromatography flame ionization detector,GC-FID)2种方法确定主成分含量。水分、挥发性有机溶剂与无机元素杂质分别采用卡尔费休滴定法、顶空气相色谱-质谱联用和电感耦合等离子体质谱法测量。结果主成分含量扣除相应杂质之后得到标准物质纯度值99.7%。标准物质不确定度是合成稳定性、均匀性、HPLC和GC主成分定值、水分、挥发性有机成分(volatile organic compound,VOC)和无机元素结果等不确定度,扩展不确定度为0.5%(k=2)。结论该方法能够进行三甲基吡嗪的准确定值,且标准物质的均匀性、稳定性良好。Objective To establish a method for purity determination and uncertainty evaluation of 2,3,5-trimethylpyrazine reference material. Methods The qualitative analysis was performed by gas chromatographymass spectrometry（GC-MS）, fourier transform infrared spectroscopy（FT-IR） and nuclear magnetic resonance（NMR）. To enhance the accuracy of the purity determination, the content determination of the main component was carried out by the high performance liquid chromatography-diode array detector（HPLC-DAD） and gas chromatography flame ionization detector（GC-FID）. The content of moisture, other inorganic elements and residual solvent were also determined by Karl Fischer coulometric method, inductively coupled plasma mass spectrometry and headspace gas chromatography-mass spectrometry, respectively. Results The purity of the reference material was 99.7% after deducting the corresponding impurities from principal component. The standard material uncertainty was the uncertainty of synthetic stability, uniformity, HPLC and GC principal components, water, volatile organic compound（VOC） and inorganic element results, and the extended uncertainty was 0.5%（k=2）. Conclusion The method can be used for the determination of 2,3,5-trimethylpyrazine, and the reference material has good uniformity and stability.

关 键 词：三甲基吡嗪 液相色谱法 气相色谱法 不确定度 

分 类 号：TQ421.31[化学工程]