聚合物添加剂的超临界流体色谱分析

SFC已被很好地用于手性药物分离和纯化，最近也被用于非手性药物化合物。随着SFC柱技术的不断探索，SFC正被应用于各种行业，分析比以往更广泛的化合物。使用HPLC的典型聚合物添加剂分离可能需要40分钟以上。如果SFC能够成功地应用于聚合物添加剂分离，那么它的速度应该能够显著减少分析时间。Application Note 2/3The Analysis of Polymer Additives using Supercritical Fluid Chromatography The Analysis of Polymer Additives using Supercritical Fluid Chromatography SFC has been well established for chiral pharmaceutical separations and puri f ications and has also recently been ut i lized for achiral pharmaceutica l compounds . As SFC column technology continues to be explored， the SFC is being appl i ed to various industries analyz i ng a wider range of compounds that ever before. A typical polymer additive separ a tion using HPLC can take upwards of 40 minutes. The s p eed of SFC should be able to significantly reduce that analysis time if it can successfully be applied to polymer addi ti ve separations. Keywords： SFC， Polymer Additives， C18 column， UV Detector，Irgafos 168， I rgafos 168 phosphate ， Tinuv i n 327， Chimassorb 81 Application Note E xperimenta l Equipment Co nd i t i ons CO， Delivery Pump： PU-2080-CO. Column： Autosampler： AS-2059-SF CO， Flowrate： UV Wavelength： Column Oven： CO-2060 CO， Flowrate： UV Detector： UV-2075 Back Pressure Regulator： BP-2080 Column Temperature： R esu l ts Fi gu r e 1. S t ack chromatogram s of Ti n uv i n 327 (6u g/u L) ，Ir g afos 168 (4ug/u L)， Ir g afos 168 Phosphate (8ug /u L ) and Chimassorb 81 (10ug /u L). C o n ditions： Colum n Luna C18 (150x4.6 m m ， 5um ) ， Flow rate 3m L s /m in (100% CO 2)， T em p erature 40C ， Back Pr ess u re G r a d ie n t 150ba r to 250ba r ove r 4 mi n utes， 220nm ， 50uL I n jection each. At t hese concent r at i ons t h e detecto r was c l earl y over l oaded with signal . The chromatogram of the 4 polymer additive standards separated using a pressure gradient is shown in figure 1. As seen the concentration of each was too high and thus t he concentration of each was reduced when a mixture of t he 4 was created. Figure 2 shows t he separation of that mixt u re using a solvent gradi e n t ， wh i le figure 3 shows the separation using the same pressure gradient used in figure 1. Figur e 2. Chrom a togram o f T in uv in 327 (0.8ug /u L )， I r gafo s 168 (1.5ug/uL )， I rgaf o s 168 Ph os phat e (3u g/uL) a nd C h i m a s s o rb 81mixt u re (0.8ug /uL) i n A ce ton e . Con d i t i on s ： Col u mn Lun a C18 (150x4.6 m m， 5um)， Fl ow ra t e 3m L s/m in (Gr ad 0% t o 20%Met hano l o v e r 6 min ut e s)， T e m p e ra tu re 40C， B ac k Pr essure 150b ar， 220n m， 15u L I nje ct i on . Fig ur e 3.Chromato gr a m of Ti n u v i n 327 (0.8u g /uL)， I r ga f os 168 (1.5u g /u L)， I r ga f os 168 Ph os p hate (3ug/u L ) and Ch i massorb 81 m ix t u r e (0.8ug /uL) in Acetone . Condit i ons： Col u m n L u n a C 18 (150x4.6 mm ， 5um) ， F l ow rate 3mLs/m i n (100% CO2)，T emperat u re 40C ， Back Pr essure G r adient 150bar to 200bar over 4 m i n utes， 220nm， 10u L I n jection. Concl u sion SFC successfully sepa r atedlrgafos 168， Irgafos 168 phosphate， T inuvin 327 and Chimassorb 81 using only CO2 as the mobile phase on a C18 column.