毛细管气相色谱法测定舒必利中有机溶剂残留量

目的：建立气相色谱法测定舒必利中3种有机溶剂的残留量的方法.方法：采用HP-1毛细管色谱柱（30.0 m×0.53 mm,5μm）;进样口温度为205℃;FID检测器温度为280℃;柱温：程序升温,60℃保持5 min,然后以20℃·min-1的速率升温120℃,保持5 min;以氮气为载气,载气流速为3.0 ml· min-1;直接进样,进样量为1μl;以N,N-二甲基甲酰胺为溶剂.结果：甲醇,乙醇和乙二醇及溶剂峰彼此均能良好分离,线性范围分别为1.51 ～ 301.72 μg·ml-1（r =0.999 9）,1.51 ～ 502.56μg·ml-1（r =0.999 9）,4.11～65.76 μg·ml-1（r =0.999 1）;平均回收率分别为93.6％,91.7％,92.8％,RSD分别为2.5％,3.0％,5.7％（n=9）.结论：该法准确可靠,适用于舒必利中这3种有机溶剂残留量的测定.

Determination of Residual Organic Solvents in Sulpiride by Capillary GC

Objective：To establish a method for the determination of three residual organic solvents in sulpiride.Methods：The determination was carried out with an HP-1 capillary column （30.0 m ×0.53 mm,5 μm） and an FID detector.The inlet temperature was 205℃ and the detector temperature was 280℃.The column temperature was with programmed temperature：the initial temperature was 60℃,maintained for 5 min,raised to 120℃ with a rate of 20℃ · min-1,and maintained for another 5 min.The carries gas was nitrogen with the flow rate of 3.0 ml · min-1,the direct injection was used with the injection volume of 1 μl.N,N-Dimethylformamide was used as the solvent.Results：Methanol,ethanol and ethyleneglycol could be separated from the solvent.The calibration curve was linear within the range of 1.51 ～ 301.72 μg · ml-1 （r =0.999 9）,1.51 ～ 502.56 μg · ml-1 （r =0.999 9） and 4.11 ～ 65.76 μg ·ml-1 （r =0.999 8）,respectively.The average recovery was 93.6%,91.7 % and 92.8 % with RSD of 2.5 %,3.0% and 5.7 % （n =9）,respectively.Conclusion：The method can be applied in the determination of the three residual organic solvents in sulpiride.