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建立液固顶空气相色谱法分析阿立哌唑中溶剂残留。采用DB-FFAP大口径毛细管柱,以正丙醇为内标进行定量。正己烷、二氯甲烷、乙醇、乙腈的线性范围分别为2.5 ~ 248.0μg·ml-1 (r=0.9991),4.5~ 452.0μg.ml-1(r=0.9999),3.9~ 386.0μg·ml-1 (r=0.9992),3.0~296.0μg·ml-1(r=0.9994),回收率分别为96.77%,97.12%,107.11%,101.35%,RSD分别为2.72%,1.15%,2.06%,1.02%。最低检测限分别为0.02μg·g-1,0.04 μg·g-1,0.04 μg·g-1,0.03 μg·g-1。本方法简单,准确,灵敏度高,重现性好。
A liquid-solid headspace gas chromatography was developed for the determination of solvent residues in aripiprazole. Using DB-FFAP large-diameter capillary column, with n-propanol as internal standard for quantitative. The linear range of n-hexane, dichloromethane, ethanol and acetonitrile were 2.5 ~ 248.0μg · ml -1 (r = 0.9991), 4.5 ~ 452.0μg.ml-1 (r = 0.9999), 3.9 ~ 386.0μg · ml- The recoveries were 96.77%, 97.12%, 107.11% and 101.35%, respectively, and the RSDs were 2.72%, 1.15%, 2.06% and 1.02 respectively (r = 0.9992) and 3.0 ~ 296.0μg · ml- %. The limits of detection were 0.02μg · g-1, 0.04μg · g-1, 0.04μg · g-1 and 1.03 μg · g-1, respectively. The method is simple, accurate, high sensitivity, good reproducibility.