摘要
目的建立测定盐酸尼卡地平原料中残留溶剂含量的顶空气相色谱(GC)法。方法采用顶空进样法,色谱柱为以6%氰丙基苯、94%二甲基硅氧烷为固定液的DB-624型毛细管柱(30 m×0.32 mm,1.8μm),程序升温,检测器为火焰离子化检测器(FID)、温度230℃,载气为氮气,分流比为10∶1,进样口温度为200℃。结果甲醇、丙酮、三氯甲烷、甲苯质量浓度分别在10.409~401.278μg/m L,10.008~400.308μg/m L,9.877~88.895μg/m L,3.022~120.873μg/m L范围内与峰面积线性关系良好,r为0.994 5~0.998 7;精密度、稳定性试验结果的RSD均小于3%(n=6);平均加样回收率分别为101.62%,102.26%,101.63%,102.32%,RSD分别为3.96%,3.54%,3.26%,3.69%(n=9)。结论该方法操作简便,能用于准确测定甲醇、丙酮、三氯甲烷、甲苯的含量。
Objective To establish a headspace gas chromatography(GC)method for the content determination of residual solvents in nicardipine hydrochloride.Methods The headspace method was adopted,the chromatographic column was DB-624 capillary column(30 m×0.32 mm,1.8μm)with 6%cyanopropylbenzene and 94%dimethylsiloxane as the stationary liquid.The temperature was programmed,the detector was flame ionization detector(FID),and its temperature was 230℃,the carrier gas was nitrogen,the split ratio was 10∶1,and the injection port temperature was 200℃.Results The linear ranges of methanol,acetone,trichloromethane and toluene were10.409-401.278μg/m L,10.008-400.308μg/m L,9.877-88.895μg/m L,3.022-120.873μg/m L(r=0.9945-0.9987),respectively.The RSDs of precision and stability tests were less than 3%(n=6).The average recoveries of methanol,acetone,trichloromethane and toluene were 101.62%,102.26%,101.63%and 102.32%with RSDs of 3.96%,3.54%,3.26%and 3.69%(n=9),respectively.Conclusion The method is simple,which can be used for the accurate determination of methanol,acetone,trichloromethane and toluene.
作者
罗晶
柳小秦
安学霞
戴涌
李霞
魏亚宁
LUO Jing;LIU Xiaoqin;AN Xuexia;DAI Yong;LI Xia;WEI Yaning(Shaanxi Institute for Food and Drug Control,Xi'an,Shaanxi,Chinn 710065)
出处
《中国药业》
CAS
2021年第6期44-46,共3页
China Pharmaceuticals
基金
陕西省重点研发计划项目[2018SF-100]。
关键词
气相色谱法
甲醇
丙酮
三氯甲烷
甲苯
盐酸尼卡地平
残留溶剂
含量测定
gas chromatography
methanol
acetone
trichloromethane
toluene
nicardipine hydrochloride
residual solvents
content determination
