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（30.0 m×0.25 mm×0.25 μm）；柱温（程序升温）：50 ℃维持5 min，以8℃/min的升温速率升温至220 ℃，再维持5 min；进样口温度250 ℃；FID检测器温度250 ℃；1％甲醇的0.1 mol/L氢氧化钠水溶液为溶解介质，载气为氮气，体积流量1.0 mL/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＝0.990 7～0.999 4，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。

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?C (holding for 5 min), then elevating to 220 ?C with the increasing rate of 8 ?C/min (holding for another 5 min); Both the injector and FID detector temperatures were 250 ?C; 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.

“十一五”国家科技支撑计划资助项目（2007BAI41B06）