HPLC测定WF-1中间体M1中的丁二酰亚胺  

Determination of succinimide in intermediate M1 of WF-1 by HPLC

作　　者：王亚楠 程旖 许嘉芮 付春梅[1] 刘秀秀[1] 晁若冰[1] WANG Yanan;CHENG Yi;XU Jiarui;FU Chunmei;LIU Xiuxiu;CHAO Ruobing(West China School of Pharmacy,Sichuan University,Chengdu,Sichuan,610041 P.R.China)

机构地区：[1]四川大学华西药学院,四川成都610041

出　　处：《华西药学杂志》2022年第5期556-558,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的 采用HPLC法测定WF-1中间体M1中N-溴代丁二酰亚胺(NBS)的残留量。方法 采用Packed C色谱柱,流动相为0.02 mol·L磷酸二氢钾水溶液-甲醇,梯度洗脱,检测波长210 nm。NBS在水溶液中转化为丁二酰亚胺,通过测定丁二酰亚胺的含量,换算NBS在样品中的残留量。结果 丁二酰亚胺与样品中其他组分的分离度良好;5~50μg·mL丁二酰亚胺的峰面积与浓度的线性关系良好(r=0.9994);检测限和定量限分别为0.01、0.04μg·mL;进样精密度和日内精密度的RSD均小于1.0%;加样回收率为93.5%。结论 所用方法专属性好、结果准确,可用于WF-1中间体M1中丁二酰亚胺的含量测定,为样品中NBS残留量的评估提供了依据。OBJECTIVE To determine the residual N-bromosuccinimide(NBS) in intermediate M1 of WF-1 by HPLC.METHODS It was conducted on a Packed column Cwith 0.02 mol·Lpotassium phosphate monobasic aqueous solution and methanol eluting in a gradient program.The detection wavelength was set at 210 nm.According to the conversion of NBS into succinimide in aqueous solution, the contents of NBS in samples were evaluated by determining the succinimide.RESULTS Succinimide was completely separated from the other components in samples.The range of linear regression for succinimide was 5-50 μg·mL,with a good related coefficient(r=0.9994).The detection limit and quantitation limit of succinimide were 0.01 μg·mLand 0.04 μg·mL,respectively.The RSD of peak area of injection precision and intra-day precision were both less than 1.0%.The mean recovery was 93.5%.CONCLUSION The method is specific, accurate, which can be used to determine succinimide and to evaluate the residual NBS in M1 of WF-1.

关 键 词：WF-1 中间体M1 丁二酰亚胺 N-溴代丁二酰亚胺 含量测定 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]