摘要
提出了顶空-气相色谱法测定吡罗昔康原料药中残留的4种有机溶剂（乙醇、丙酮、氯仿和甲苯）的方法。分别选择65℃及30min作为样品在顶空瓶中的平衡温度和平衡时间。选用RtX-1毛细管色谱柱（0．25mm×30m，0．25μm）分离，氢火焰离子化检测器测定。4种有机溶剂在10min内能完全分离，分离度大于1．5。4种有机溶剂的质量浓度在一定的范围内与其峰面积呈线性关系，检出限（3S／N）在0．043-0．114mg·L-1之间。方法用于吡罗昔康原料药样品分析，仅检出残留溶剂乙醇和丙酮。加标回收率在98．1％～101．7％之间。
Four residual organic solvents, including ethanol, acetone, chloroform and toluene, in raw medicinal piroxicam were determined by head-space GC. The temperature and time chosen for equilibration of the sample in the head space vessel were 65℃ and 30 min respectively. Capillary chromatographic column, Rtx-1 （0. 25 mm×30 m, 0. 25 μm） was used for the separation, and hydrogen FID was adopted in the determination. Under the optimum conditions, the 4 organic solvents were separated within 10 min, and the separation factor attained was more than 1. 5. Linear relationships between values of peak area and mass concentration of the 4 organic solvents were obtained in definite ranges, with detection limit （3S/N） in the range of 0. 043 0. 114 mg · L-1. The proposed method was applied to the analysis of raw medicinal piroxicam, both ethanol and acetone was detected. Values of recovery found by standard addition method were ranged from 98.1% to 101.7%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第9期1060-1062,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
顶空-气相色谱法
吡罗昔康
原料药
有机溶剂
Head-space gas chromatography
Piroxicam
Raw medicinal
Organic solvent
作者简介
彭炳先（1970-），男，江西南昌人，硕士，讲师，研究方向为药物分析。
