顶空气相色谱法测定布南色林残留溶剂的含量

Determination of Residual Solvent in Blonanserin by Gas Chromatography with Headspace Sampling

摘要：目的建立气相色谱法测定布南色林中残留溶剂含量的方法。方法采用6％氰丙基苯基-94％二甲基聚硅氧烷为固定液的毛细管柱（DB-624，0．53mm×30m，3．0μm），程序升温，初始温度50℃，保持5min，以20℃／min的速率升温至200℃，保持5min；氢火焰离子化检测器（FID），检测器温度250℃，进样口温度220℃，载气为氮气，流速2mL／min，进样体积1mL。外标法计算残留溶剂的含量。结果5种有机溶剂进样浓度与峰面积呈良好线性关系，相关系数均大于0．9990，加样回收率在97．6％～102．9％之间。结论此法准确可靠，灵敏度高，可用于布南色林中残留溶剂的测定。

Objective To establish a GC method for the determination of residual solvents in blonanserin. Methods DB-624 chromatographic column （coated with 6 % cyanopropylphenyl-94 % dimethylpolysiloxane, length 30 m, I.D. 0.53 mm, film 3.0μm） was adopted. The column temperature was programmed： kept at 50℃ for 5 min, and then increased by 20℃/min to 200℃ for 5 min, and keot for 5 min. The temperature of FID detector was 250℃ and the temperature of inlet was 220℃. The carrier gas was nitrogen at a flow rate of 2 mL/min. The injection volume was 1 mL. Contents of residual solvents were calculated according to the external standard method. Results The calibration curves of five solvents all showed good linearity in a detected concentration range（r〉0.9990）, the range of average recovery was 97.6 %-102.9 %. Conclusion The method was accurate, reliable and sensitive, and can be used for assay of residual organic solvents in blonanserin.