液固顶空气相色谱法测定阿立哌唑中溶剂残留

Determination of Residual in Aripiprazole by Solution-Solid Headspace Gas Chromatography

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-1,0.04μg·g-1,0.03μg·g-1.本方法简单,准确,灵敏度高,重现性好.

To develop solution-solid headspace gas chromatography for the determination of residual solvent in Aripiprazole. UsingDB-FFAP Wide Bore capillary column and propanol as internal standard.The linear concentration region of n-hexane was 7.9~ 317.0μg·ml-1 (r=0.9996), dichloromethane was 0.7~35.5μg·ml-1 (r=0.9998),ethanol was 1.5~73.5μg·ml-1 (r=0.9992), acetoni-trile was 0.9~44.4μg·ml-1 (r=0.9994),the relative recovery of n-hexane was 101.64﹪, dichloromethane was 97.18﹪, ethanol was99.32%, acetonitrile was 101.12 %,with RSD 1.97﹪, 1.10﹪, 2.40﹪and 0.84﹪respectively. The lowest test limits of n-hexane,dichloromethane,ethanol and acetonitrile are respectively 0.02 μg·g-1,0.04 μg·g-1,0.04 μg·g-1,0.03 μg·g-1. The method issimple, accurate, highly sensitive and of good reproducibility.