摘要
目的建立TM-2中9种有机溶剂残留量测定法。方法采用气相色谱法,色谱柱为DB-624（30 m×530μm,3μm）毛细管柱,程序升温,检测器为FID,载气为氮气;采用顶空进样法,平衡温度为115℃,平衡时间为20 min。结果甲醇、乙腈、二氯甲烷、叔丁醇、正己烷、乙酸乙酯、四氢呋喃、三乙胺及吡啶线性关系良好（r≥0.992 9）,平均回收率为89.9%--102.4%（RSD=3.6%）,检测限分别为0.28、0.30、0.53、0.22、0.03、0.07、0.05、0.15、0.15 mg·L-1。结论本方法可用于TM-2原料药中残留溶剂的检查。
Objective To develop a method for determination of nine kinds of residual solvents in TM-2 by headspace gas chromatography. Methods The residual solvents were separated on DB-624（ 30 m × 530 μm,3 μm） capillary chromatography column using temperature programming. Nitrogen gas was used as carrier gas with FID as detector. Results There were good linear relationships in the experimental concentrations of methanol,acetonitrile,dichloromethane,tert-butylalcohol,n-hexane,ethyl acetate,tetrahydrofuran,triethylamine,pyridine（ r ≥ 0. 992 9）. The average recoveries were ranged from 89. 9% to 102. 4%（ RSD =3. 6%）. The limit of detection were 0. 28,0. 30,0. 53,0. 22,0. 03,0. 07,0. 05,0. 15 and 0. 15 mg·L- 1,respectively. Conclusions The method is simple,sensitive and accurate. It could be used for detection of residual solvents in TM-2.
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2015年第7期523-526,536,共5页
Journal of Shenyang Pharmaceutical University
