反相高效液相色谱法测定合成反应产物中溴代硝基芴酮

提出了用反相高效液相色谱法测定合成溴代硝基芴酮类化合物的反应产物中2,7-二溴-4-硝基芴酮(DBNFN)的含量。样品用甲醇作溶剂超声溶解,以Elite Hypersil ODS2C18色谱柱及甲醇-水(85+15)混合溶液作流动相进行分离。在所选择的条件下可达到DBNFN与共存物2,7-二溴芴酮(合成所用原料)和芴酮衍生物(副产品)三者之间的完全分离。采用紫外检测(波长254nm)和外标法定量。DBNFN的质量浓度在0.1～2.5g.L-1范围内与其峰面积呈线性关系。方法的检出限(2S/N)为3.8μg.L-1。用标准加入法做回收试验,测得回收率在99.2%～99.8%之间,测定值的相对标准偏差(n=6)在0.35%～0.48%之间。

RP-HPLC Determination of Bromonitrofluorenones in the Reaction Products of Synthesis

RP-HPLC was applied to the determination of 2,7-dibromo-4-nitrofluorenone(DBNFN) in the reaction products of synthesis of bromonitrofluorenones.Sample was dissolved in methyl alcohol ultrasonically.Elite Hypersil ODS2 C18 chromatographic column and mixture of CH3OH+H2O(85+15) were used as mobile phase for separation.Under the optimized conditions,complete separation of DBNFN from the raw material of 2,7-dibromofluorenone and the derivatives of fluorenone(as by-products) was attained.UV detection at 254 nm and external standard calibration were adopted for determination of DBNFN.Linear relationship between values of peak area and mass concentration of DBNFN was obtained in the range of 0.1-2.5 g·L-1.Detection limit(2S/N) found was 3.8 μg·L-1.Values of recovery found by standard addition method were in the range of 99.2%-99.8%,with values of RSD′s(n=6) ranged from 0.35% to 0.48%.