UHPLC-QTOF-MS高效检测CL-20合成过程的杂质

UHPLC⁃QTOF⁃MS High Efficiency Eetectionof Impurities in a Typical CL⁃20Synthesis Process

为了快速准确检测和分析六硝基六氮杂异伍兹烷(CL-20)合成过程中产生的中间体和杂质,控制CL-20纯度或品质,保证其感度及爆轰性能,采用核磁共振(NMR)和超高高效液相色谱-四极杆飞行时间质谱(UHPLC-QTOF-MS)技术快速、高效分析检测了CL-20典型合成工艺过程中组分及杂质。结果表明,六苄基六氮杂异伍兹烷(HBIW)中的杂质为1,3-二苄基咪唑,四乙酰基二苄基六氮杂异伍兹烷(TADB)中的杂质为低酰基化的三乙酰基三苄基六氮杂异伍兹烷(TATB),四乙酰基六氮杂异伍兹烷(TAIW)中的杂质为未完全反应的TADB,CL-20中的杂质为未完全硝化的一乙酰基五硝基六氮杂异伍兹烷(MPIW)和二乙酰基四硝基六氮杂异伍兹烷(DATN)。

Quickly and accurately detect and analyze the intermediates and impurities produced in the synthesis of Hexanitro-hexaazaisowurtzitane(CL-20),is important for controlling the purity or quality of CL-20,and ensuring its sensitivity and detona-tion performance.In this study,nuclear magnetic resonance(NMR)and ultra-high performance liquid chromatography-Quadrupole time-of-flight mass spectrometry(UHPLC-QTOF-MS)were used to rapidly and efficiently analyze the impurities in the typical synthesis process of CL-20.The results showed that the impurity in HBIW was 1,3-dibenzyl imidaz-ole,the impurity in tetraacetyl dibenzyl hexazepane(TADB)was low acylated triacetyl tribenzyl hexazepane(TATB),and the impurity in tetraacetyl hexazepane(TAIW)was incomplete TADB.The impurities in CL-20 were not fully nitrated monoacetyl pentanitrohexazazine(MPIW)and diacetyl tetranitrohexazazine(DATN).