顶空气相色谱法测定阿可拉定（IC162）中大孔树脂有机溶剂残留物

目的：建立阿可拉定中9种大孔树脂有机溶剂残留物的检测方法。方法：采用顶空进样毛细管气相色谱法,色谱柱为HP-INNOWAX毛细管柱（30.0m×0.25mm×0.25μm）;柱温（程序升温）：50℃维持5min,以8℃/min的升温速率升温至220℃,再维持5min;进样口温度250℃;FID检测器温度250℃;1%甲醇的0.1mol/L氢氧化钠水溶液为溶解介质,载气为氮气,体积流量1.0mL/min,测定阿可拉定中正己烷、苯、甲苯、邻二甲苯、对二甲苯、苯乙烯、二乙基苯、二乙烯基苯、正十二烷9种大孔树脂有机溶剂残留量。结果：本法线性关系良好,r=0.9907～0.9994,RSD均小于8.3%,9种溶剂的平均回收率为77.1%～105.4%,其RSD〈6.0%。结论：该方法操作简便快速,灵敏度高,准确度好,可作为阿可拉定中大孔树脂有机溶剂残留量的测定方法。

Detection of organic solvent residues of macroporous resin in IC162 by headspace gas chromatography

Objective：To establish a method for detecting the nine kinds of organic solvent residues of macroporous resin in IC162.Methods：Headspace capillary gas chromatography with HP-INNOWAX column（30.0 m × 0.25 mm × 0.25 μm） was used to determine the residues of macroporous resin in IC162;The initial temperature of column temperature program was 50℃（holding for 5 min）,then elevating to 220 ℃ with the increasing rate of 8 ℃/min（holding for another 5 min）;Both the injector and FID detector temperatures were 250 ℃;Solvent media was 1% methanol with 0.1 mol/L sodium hydroxide solution and the carrier gas was nitrogen;Flow velocity was 1.0 mL/min,nine kinds of organic solvent residues of macroporous resin in IC162 were detected,such as n-hexane,benzene,methylbenzene,o-xylene,p-xylene,styrene,diethylbenzene,divinylbenzene,and dodecanetotal.Results：There was a good linearity of headspace gas chromatographic method（r = 0.990 7-0.999 4）,the RSDs of precision were all less than 8.3%.The average recoveries of the nine residues were in the range of 77.1%-105.4% and their RSDs were all less than 6.0%.Conclusion：The method is simple,accurate,and sensitive.It can be used for the detection of organic solvent residues of macroporous resin in IC162.