首页> 中文期刊> 《应用化工》 >液相色谱法测定2-{2-叔丁基-6-2-(1,1,7,7-四甲基-2,3,6,7-四氢-1H,5H-吡啶并3,2,1-ij喹啉-9-基)-乙烯基-吡喃-4-内鎓盐烯}-丙二腈的纯度

液相色谱法测定2-{2-叔丁基-6-2-(1,1,7,7-四甲基-2,3,6,7-四氢-1H,5H-吡啶并3,2,1-ij喹啉-9-基)-乙烯基-吡喃-4-内鎓盐烯}-丙二腈的纯度

         

摘要

Propanedinitrile , [ 2- ( 1 , 1 -dimethylethyl) -6-[ 2-( 2, 3 , 6, 7-tetrahydro-1 , 1 , 7 , 7-tetramethyl-1H ,5H-benzo [ij] quinolizin-9-yl) ethenyl] -4H-pyran-4-ylidene] ( DCJTB) was determined by HPLC. Analytical conditions of sample preparation , mobile phase and detect wavelength were tested and optimized. Method of external standard method was used in the determination. The results showed that sample should be taken from many spots, dissolved and evaporated. The mobile phase was THF-H2O (mixed in the ratio of 65∶35). Detect wavelength was 360 nm and 296 nm was auxiliary. Precision and recovery of the method were tested,giving results of recovery in the range of 99.9% ~ 101. 2% , and value of RSD (n =5) of 1.1%. DL of the method was 1.1 × 1O -5s g/L and linearity was observed in range of 0. 08 ~ 0. 97 mg/ml.with correlation coeffieient of 0. 998 9. RSD of determination was 1.1 %' ( n = 5) . The method was applied to actual samples.%建立了2-{2-叔丁基-6-[2-(1,1,7,7-四甲基-2,3,6,7-四氢-1H,5H-吡啶并[3,2,1-ij]喹啉-9-基)-乙烯基]-吡喃-4-内鎓盐烯}-丙二腈(简称DCJTB)的反相高效液相色谱法检测方法,讨论了样品制备的影响因素及流动栩与检测波长的选择,计算了回收率和精密度,并采用外标法对其标准溶液进行了测定.结果表明,样品制备时应多点采集,然后溶解挥干:流动相四氢呋喃∶水(体积比)=65∶35;360 nm作为检测波长,同时用296 nm作为参考检测波长;DCJTB回收率为99.9%~101.2%,精密度RSD=1.1%(n=5),最小检测量为1.1×10~g/L,线性范围0.08~0.97 mg/mL,线性相关系数为0.998 9.此方法简便、准确、重现性好.

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