摘要
为建立测定恩扎卢胺原料药中三氯甲烷和四氯化碳残留的方法,设计采用HP-5毛细管色谱柱(30 m×0.320 mm,0.25μm),气相色谱载气为氮气,载气流速为1.0 mL/min,顶空进样,选用电子捕获(ECD)检测器,进样口温度为250℃,检测器温度为300℃。结果表明:三氯甲烷、四氯化碳质量浓度分别在0.0599~11.9720μg/mL,0.0042~0.8454μg/mL范围内,线性关系良好(r均大于0.995);检测限分别为18.0 ng/mL、1.3 ng/mL;定量限分别为59.9μg/mL、4.3μg/mL;平均回收率分别为104.89%、102.77%,RSD分别为6.91%、5.12%(n=9);精密度试验的RSD为6.24%和6.70%(n=6)。证明该方法灵敏度高、准确度好、且操作便捷,可用于检测恩扎卢胺原料药中三氯甲烷和四氯化碳溶剂残留。
To establish a method for determining of residual trichloromethane and carbon tetrachloride in Enzalutamide raw materials.HP-5 capillary chromatography column(30 m×0.320 mm,0.25μm)was used,carrier gas of nitrogen,carrier gas flow rate of 1.0 mL/min,headspace injection,ECD detector was designed,inlet temperature of 250℃,detector temperature of 300℃.The results show that the mass concentrations of trichloromethane and carbon tetrachloride were 0.0599~11.9720μg/mL,0.0042~0.8454μg/mL,the linear relationship is good(r is greater than 0.995).The detection limits are 18.0 ng/mL and 1.3 ng/mL,respectively.The quantification limits are 59.9 ng/mL and 4.3 ng/mL.The average recovery rates were 104.89%and 102.77%,respectively,with RSDs of 6.91%and 5.12%(n=9).The RSD for precision testing is 6.24%and 6.70%(n=6).This method is has good sensitivity,high accuracy and simple to operate,and can be used to detect residual solvents of trichloromethane and carbon tetrachloride in Enzalutamide raw materials.
作者
王红芳
游蓉丽
宋小飞
杨玲玲
WANG Hong-fang;YOU Rong-li;SONG Xiao-fei;YANG Ling-ling(Shanxi Zhendong Pharmaceutical Co,Ltd.,Changzhi 046000,China)
出处
《安徽化工》
2025年第2期144-148,共5页
Anhui Chemical Industry
基金
山西省科技成果转化引导专项(202204021301013)。
关键词
顶空-气相色谱法
恩扎卢胺
三氯甲烷
四氯化碳
质量控制
headspace gas chromatography
Enzalutamide
trichloromethane
carbon tetrachloride
quality control
