DNTF纯度标准物质中有机杂质HPLC–QQQ–MS法定值

Determination of organic impurities in DNTF purity reference material by HPLC–QQQ–MS

利用气质联用(GC–MS)、液质联用(LC–MS)和核磁共振(NMR)对3,4-二硝基呋咱基氧化呋咱(DNTF)粗品中的有机杂质进行鉴别研究,解析各杂质可能的结构。利用LC–MS确定精制后DNTF标准物质中的杂质为双呋咱并(b,f)氧化呋咱氧杂环庚三烯(BFT)和三呋咱并氧杂环庚三烯(TFO),合成出两种杂质对其结构进行了确认验证。采用高效液相色谱–三重四极质谱(HPLC–QQQ–MS)对有机杂质BFT和TFO定值,BFT和TFO的定量限分别为55ng/g和15ng/g;BFT和TFO的质量浓度在1～100ng/mL范围内与其色谱峰面积均呈良好的线性关系,相关系数分别为0.999 4,0.999 2;定值方法的相对标准偏差(RSD)小于3.5%(n=6)。BFT的定值结果为0.006%,TFO的定值结果 0.004%。与液相色谱、气相色谱等测定方法相比,建立的方法具有定量限低、准确度高和定值精度高等优点。

The organic impurities in 3,4-dinitrofurazanfuroxan(DNTF)coarse products were identified by GC– MS,LC–MS and NMR,and the possible structures of various impurities were analyzed.The impurities in the refined DNTF reference material were bisfurazone(b,f)oxatrioxane(BFT)and trifurazanoxine(TFO)determined by LC–MS,the structures were synthesized to confirm and verify.HPLC–QQQ–MS was used to determine the two impurities.The quantitation limits of BFT and TFO were 55 ng/g and 15 ng/g,respectively.The mass concentration of BFT and TFO were linear with its chromatographic peak area in the linear range of 1–100 ng/mL,the correlation coefficients were 0.999 4,0.999 2,respectively.The relative standard deviation of the determination results was less than 3.5%(n=6).The detection result was 0.006%for BFT,and 0.004%for TFO.Compared with liquid chromatography and gas chromatography,this method has the advantages of low limits of quantitation,the high accuracy and the high precision.