摘要
目的建立测定盐酸那拉曲坦起始原料吲哚-5-甲醛中残留溶剂含量的气相色谱法。方法采用DB-WAX毛细管色谱柱(30 m×0.25 mm,0.25μm),溶液直接进样,以二甲基亚砜为溶剂,程序升温,载气为氮气,流速为1.0 mL·min^(-1),氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃,分流比为20∶1。结果乙醇、甲苯、吡啶、二甲基甲酰胺、二甲基乙酰胺和乙酸的线性范围分别为20.02~600.5(r=0.9999)、3.588~107.6(r=0.9998)、0.8016~24.05(r=0.9999)、3.518~105.5(r=0.9999)、4.366~131(r=0.9998)、20.08~602.3(r=0.9995)μg·mL^(-1);平均回收率在97.4%~98.5%,RSD在0.88%~6.1%;定量限在0.72~20μg·mL^(-1),检测限在0.36~10μg·mL^(-1)。结论本法简便、准确、重复性好,可用于吲哚-5-甲醛中残留溶剂的检测。
Objective To determine the residual organic solvents in indole-5-formaldehyde the starting material of naratriptan hydrochloride by gas chromatography.Methods The residual organic solvents were separated on a DB-WAX capillary chromatographic column(30 m×0.25 mm,0.25μm)with temperature programming.Nitrogen was used as the carrier gas at the flow rate of 1.0 mL·min^(-1).The temperature of injector was 200℃.A flame ionization detector was used at 250℃,the split ratio at 20∶1.Results The linearity was 20.02-600.5μg·mL^(-1)for ethanol(r=0.9999),3.588-107.6μg·mL^(-1)for methylbenzene(r=0.9998),0.8016-24.05μg·mL-1 for pyridine(r=0.9999),3.518-105.5μg·mL^(-1)for dimethylformamide(r=0.9999),4.366-131μg·mL^(-1)for dimethylacetamide(r=0.9998),and 20.08-602.3μg·mL^(-1)for acetic acid(r=0.9995).The average recoveries were 97.4%-98.5%,with RSD of 0.88%-6.1%.The limit of quantitation was 0.72-20μg·mL^(-1),and the limit of detection was 0.36-10μg·mL^(-1).Conclusion The method is simple,accurate and reproducible,and can be used to determine the residual organic solvents in indole-5-formaldehyde.
作者
程闽玥
王迪
金祥飞
沈卫阳
CHENG Min-yue;WANG Di;JIN Xiang-fei;SHEN Wei-yang(College of Sciences,China Pharmaceutical University,Nanjing 210009;Key Laboratory of Drug Quality Control and Pharmacovigilance,Ministry of Education,Nanjing 210009)
出处
《中南药学》
CAS
2021年第4期723-726,共4页
Central South Pharmacy
关键词
盐酸那拉曲坦
吲哚-5-甲醛
残留溶剂
气相色谱法
naratriptan hydrochloride
indole-5-formaldehyde
residual organic solvent
gas chromatography
