目的：建立阿可拉定中9種大孔樹脂有機(jī)溶劑殘留物的檢測(cè)方法。方法：采用頂空進(jìn)樣毛細(xì)管氣相色譜法，色譜柱為HP-INNOWAX毛細(xì)管柱（30.0 m×0.25 mm×0.25 μm）；柱溫（程序升溫）：50 ℃維持5 min，以8℃/min的升溫速率升溫至220 ℃，再維持5 min；進(jìn)樣口溫度250 ℃；FID檢測(cè)器溫度250 ℃；1％甲醇的0.1 mol/L氫氧化鈉水溶液為溶解介質(zhì)，載氣為氮?dú)?，體積流量1.0 mL/min，測(cè)定阿可拉定中正己烷、苯、甲苯、鄰二甲苯、對(duì)二甲苯、苯乙烯、二乙基苯、二乙烯基苯、正十二烷9種大孔樹脂有機(jī)溶劑殘留量。結(jié)果：本法線性關(guān)系良好，r＝0.990 7～0.999 4，RSD均小于8.3％，9種溶劑的平均回收率為77.1％～105.4％，其RSD＜6.0％。結(jié)論：該方法操作簡便快速，靈敏度高，準(zhǔn)確度好，可作為阿可拉定中大孔樹脂有機(jī)溶劑殘留量的測(cè)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”國家科技支撐計(jì)劃資助項(xiàng)目（2007BAI41B06）