高效液相色谱荧光检测法测定药物中的氯乙酰氯  

Determination of chloroacetyl chloride in drug substance by high performance liquid chromatography with fluorescence detection

作　　者：汤加园 陈向明[1] Tang Jiayuan;Chen Xiangming(School of Pharmacy,Binzhou Medical University,Yantai 264003,China)

机构地区：[1]滨州医学院药学院,山东烟台264003

出　　处：《化学分析计量》2021年第1期59-62,共4页Chemical Analysis And Meterage

摘　　要：建立测定药物中氯乙酰氯含量的高效液相色谱–荧光检测方法。以吖啶酮乙酰肼为荧光标记试剂,对氯乙酰氯进行柱前衍生。在室温下反应15 min,衍生产率达到最大。衍生溶液在XDB–C18柱上,以水和乙腈为流动相进行分析,激发波长和发射波长分别为255 nm和429 nm。氯乙酰氯浓度在1~1 000 nmol/L范围内与色谱峰面积具有良好的线性关系,线性相关系数r=0.999 9。方法的检出限为0.35 nmol/L,仪器精密度和方法精密度分别为0.52%和0.67%(n=6)。样品加标回收率为92.5%~95.6%。该方法简单、准确,精密度良好,可用于测定药物中氯乙酰氯的残留量。A high performance liquid chromatography method coupled with fluorescence detection to determine chloroacetyl chloride in drug substance was developed.Acridone acetyl hydrazine was used as fluorescence labeling reagent and chloroacetyl chloride was derived before column.Optimum derivatization was obtained at room temperature for 15 min.The derivative was separated on a reversed-phase XDB–C18 column in conjunction with water and acetonitrile as mobile phase.The excitation and emission wavelengths were 255 nm and 429 nm respectively.The concerntration of chloroacetyl chloride had good linear ralationship with the chromatographic peak area in the range of 1–1000 nmol/L,the linear correlation coefficient r=0.9999.The instrument precision and method precision were 0.52%,0.67%(n=6),respectively.The detection limit of the method was 0.35 nmol/L,and the recoveries were in the range of 92.5%–95.6%.The method is simple,accurate and showed good repeatability,which can be used to determine the content of chloroacetyl chloride in drug substance.

关 键 词：高效液相色谱 荧光检测 氯乙酰氯 

分 类 号：O657.7[理学—分析化学]