双膦酸盐类药物中4种有机溶剂的顶空毛细管气相色谱法测定

Determination of Residual Organic Solvents in Bisphosphonates by Headspace Capillary Gas Chromatography

以离子液体([Emim][BF4])为顶空溶剂,建立了顶空毛细管气相色谱法测定双膦酸盐类药物中甲醇、乙醇、丙酮和氯苯的残留量。采用DB-624色谱柱,FID检测器,顶空平衡温度120℃,平衡时间20min。4种有机溶剂的回收率为97.1%～100.3%,RSD均小于3.0%。检测限分别为0.15、0.06、0.06和0.007μg/ml。

An headspace capillary gas chromatography method was established for the determination of methanol,ethanol,acetone and chlorobenzene in bisphosphonates with ionic liquid as matrix medium.A DB-624 capillary column was used with temperature program and FID detector,at injection temperature 120 ℃ and equilibrium time 20 min.The recoveries were 97.1%-100.3%,with the RSDs less than 3.0%.Their detection limits were 0.15,0.06,0.06 and 0.007 μg/ml,respectively.