顶空气相色谱法测定盐酸西那卡塞的残留溶剂

Determination of Residual Solvents of Cinacalcet Hydrochloride by Headspace GC

目的建立静态顶空气相色谱法测定盐酸西那卡塞中残留的乙醇、叔丁基甲醚和甲苯。方法采用DB-624色谱柱（30m×0.32mm,0.25μm）,FID检测器。结果乙醇浓度在2.014-1007μg·mL-1范围内与峰面积呈良好的线性关系,r为1.000;叔丁基甲醚浓度在2.053-1026μg·mL-1范围内与峰面积呈良好的线性关系,r为1.000;甲苯浓度在0.4050-202.5μg·mL-1范围内与峰面积呈良好的线性关系,r为0.9998;乙醇、叔丁基甲醚和甲苯加样回收率的平均值分别为99.0%、98.0%和98.9%;RSD分别为3.4%、3.5%和3.4%。结论本方法简便、准确可靠,适用于盐酸西那卡塞中溶剂残留的控制。

OBJECTIVE To establish a headspace gas chromatograph analytical method for determining the contents of the residual solvents in cinacalcet hydrochloride. METHODS DB-642 capillary column（ 30 m ×0. 32 mm,0. 25μm） and flame ionization detection（ FID） were used. RESULTS The calibration curves were linear in the range of 2. 014 - 1007μg·mL- 1for alcohol（ r = 1. 000）; The calibration curves were linear in the range of2. 053 - 1026μg·mL- 1for tert-butyl methyl ether（ r = 1. 000）; The calibration curves were linear in the range of0. 4050 - 202. 5μg·mL- 1for toluene（ r = 0. 9998）. The average recoveries of alcohol,tert-butyl methyl ether and toluene were 99. 0%,98. 0% and 98. 9% respectively; The RSD were 3. 4%,3. 5% and 3. 4% respectively. CONCLUSION The method is simple,accurate,reliable and can be used for the quality control of residual solvents of cinacalcet hydrochloride.