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目的:建立布洛芬中有机溶剂石油醚(90~120℃)残留的测定方法。方法:采用GC-MS对布洛芬中石油醚(90~120℃)的主要组分进行定性分析,采用顶空气相色谱法(HSGC法)对石油醚(90~120℃)残留的主要组分进行测定,HP-5毛细管色谱柱(30 m×0.32 mm,0.25μm),FID检测器,程序升温,载气为氮气。结果:样品中的石油醚(90~120℃)残留主要为正己烷、2-甲基己烷、3-甲基己烷、正庚烷、2,4-二甲基己烷、2-甲基庚烷、3-甲基庚烷、正辛烷等8种成分;此8种成分在各自的浓度范围内呈良好的线性关系(r=0.997 7~0.999 6,n=5),最低检出限范围为1.50~3.10 ng·mL-1;3种加标浓度的平均回收率为95.85%~105.3%。精密度、重复性的RSD均小于5%。结论:本方法简单、灵敏、可靠,适用于布洛芬中石油醚(90~120℃)残留成分的检测。
Objective: To establish a method for the determination of petroleum ether (90-120 ℃) residues of organic solvent in ibuprofen. Methods: The main constituents of petroleum ether (90-120 ℃) in ibuprofen were qualitatively analyzed by GC-MS. The main components of petroleum ether (90-120 ℃) were analyzed by headspace gas chromatography (HSGC) The determination was carried out on a HP-5 capillary column (30 m × 0.32 mm, 0.25 μm) with a FID detector programmed temperature and a carrier gas of nitrogen. Results: The residues of petroleum ether (90-120 ℃) in the sample were mainly hexane, 2-methylhexane, 3-methylhexane, n-heptane, 2,4-dimethylhexane, (N = 5), n-heptane, 3-methylheptane and n-octane. The lowest concentrations of these eight components were found in the range of concentration (r = 0.997 7-0.9999 6, n = 5) The limit range was 1.50 ~ 3.10 ng · mL-1. The average recoveries of the three spiked samples ranged from 95.85% to 105.3%. RSD of precision and repeatability are less than 5%. Conclusion: The method is simple, sensitive and reliable and is suitable for the determination of residual components in petroleum ether (90-120 ℃) in ibuprofen.