摘要
目的:建立了测定二氟泼尼酯原料药中甲苯、二氯甲烷、正己烷、乙酸乙酯与乙醇残留量的方法。方法:采用毛细管气相色谱法。色谱柱:HP-5毛细管柱;柱温:35℃保持5min,再以50℃/min的速率升温至200℃,保持5min;氢火焰离子化检测器温度:250℃;载气:高纯氮气,流速:30ml/min;进样口温度:200℃,分流比:10:1,顶空进样;以N,N-二甲基甲酰胺为溶剂。结果:甲苯、二氯甲烷、正己烷、乙酸乙酯与乙醇在检测质量浓度范围内r值均≥0.9990,平均回收率分别为95.2%(RSD=1.07%)、96.7%(RSD=1.76%)、94.9%(RSD=1.98%)、96.1%(RSD=1.95%)、96.1%(RSD=1.12%),定量限分别为0.445、0.36、0.116、0.5、0.125ng,检测限分别为0.178、0.06、0.029、0.15、0.04ng。3批样品中只检出乙酸乙酯。结论:建立的方法灵敏、准确,可用于二氟泼尼酯原料药中5种有机溶剂的残留量测定。
OBJECTIVE：To establish a method for the determination of residual methylbenzene,dichlormethane,n-hexane,acetic ether and alcohol in difluprednate crude drug.METHODS：Capillary gas chromatography method was adopted.The determination condition was as follows：HP-5 capillary column;column temperature of 35 ℃ at 5 min,increasing to 200 ℃ at rate of 50 ℃/min,maintaining for 5 min;flame ionization detector temperature of 250 ℃;high purity nitrogen as carrier gas;flow rate of 30 ml/min;injector temperature of 200 ℃;split ratio of 10：1;headspace sampling;N,N-dimethylfomamide as solvent.RESULTS：The r in linear ranges of methylbenzene,dichlormethane,n-hexane,acetic ether and alcohol were all ≥0.999 0;average recovery were 95.2%（RSD=1.07%）,96.7%（RSD=1.76%）,94.9%（RSD=1.98%）,96.1%（RSD=1.95%）and 96.1%（RSD= 1.12%）,respectively.The limits of quantitation were 0.445,0.36,0.116,0.5 and 0.125 ng,and detection limits were 0.178,0.06,0.029,0.15 and 0.04 ng.Only the acetic ether was detected in 3 batches of samples.CONCLUSIONS：The established method is sensitive and accurate for the residual determination organic solvents in difluprednate crude drug.
出处
《中国药房》
CAS
CSCD
2013年第29期2750-2751,共2页
China Pharmacy
基金
山东省科学技术发展计划项目资助(No.2011GSF12106)
关键词
二氟泼尼酯
有机溶剂
毛细管气相色谱
残留量测定
Difluprednate
Organic solvents
Capillary gas chromatography
Residual determination
作者简介
副主任药师。研究方向：新药研发。电话：0531．81213291。E—mail：jnfengguangling@163．com．cn
