静态顶空气相色谱法测定盐酸西那卡塞中的残留溶剂  

Determination of residual solvents in cinacalcet hydrochloride by static headspace GC

作　　者：杜薇[1,2] 邹巧根[3] 孙莉莉[3] 张尊建[1,2] 

机构地区：[1]中国药科大学分析测试中心,江苏南京210009 [2]药物质量与安全预警教育部重点实验室,江苏南京210009 [3]南京工业大学生物与制药工程学院,江苏南京210009

出　　处：《华西药学杂志》2013年第3期290-292,共3页West China Journal of Pharmaceutical Sciences

摘　　要：目的采用静态顶空气相色谱分析方法测定盐酸西那卡塞原料药中残留的四氢呋喃、乙酸乙酯、二氯甲烷、乙醇和甲苯。方法采用DB-WAX色谱柱(30 m×0.32 mm,0.25μm),FID检测器,内标法定量。分别考察了溶剂、顶空平衡温度、顶空平衡时间、相比、色谱柱对残留溶剂测定的影响。结果 5种残留溶剂的线性范围分别为36～108、250～750、30～90、250～750、44.5～133.5μg.mL-1,平均回收率分别为98.2%、98.3%、98.4%、98.8%、98.1%,RSD分别为3.37%、3.36%、4.65%、2.97%、3.13%。结论所用方法简便、准确、灵敏度高、重复性好,适用于盐酸西那卡塞中残留溶剂的测定。OBJECTIVE A static headspace gas chromatograph analytical method was developed to simultaneously determinate residual solvents of tetrahydrofuran,ethyl acetate,dichloromethane,alcohol and toluene in cinacalcet hydrochloride.METHODS A DB-WAX capillary column（30 m×0.32 mm I.D.and 0.25 μm film thickness）was used under temperature programming conditions with a flame ionization detection（FID）.Quantitation was performed by internal standard analysis.The column,sample matrix,equilibrium temperature,equilibrium time and phase ratio were tested to select the optimal ones for determining the residual solvents.RESULTS The linear ranges of these solvents were 36-108,250-750,30-90,250-750,44.5-133.5 μg·mL^-1,respectively.The average recoveries were 98.2%,98.3%,98.4%,98.8% and 98.1%,with RSDs lower than 4.65%.CONCLUSION This method can be readily used to determine the residual solvents present in cinacalcet hydrochloride for it is simple,accurate,sensitive and reproducible.

关 键 词：盐酸西那卡塞 顶空气相色谱 溶剂残留 四氢呋喃 乙酸乙酯 二氯甲烷 乙醇 甲苯 

分 类 号：R917[医药卫生—药物分析学]