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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1.51~301.72μg·ml-1(r=0.999 9),1.51~502.56μg·ml-1(r=0.999 9),4.11~65.76μg·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。
Objective: To establish a method for the determination of the residues of three kinds of organic solvents in sulpiride by gas chromatography. Methods: HP-1 capillary column (30.0 m × 0.53 mm, 5 μm) was used. Inlet temperature was 205 ℃. FID detector temperature was 280 ℃. Column temperature was programmed at 60 ℃ for 5 min. The flow rate of carrier gas was 3.0 ml · min-1 with nitrogen gas as carrier gas, and the injection volume was 1μl. With N, N-dimethyl Formamide is a solvent. Results: The methanol, ethanol, ethylene glycol and solvent peaks were well separated from each other with the linear range of 1.51-301.72μg · ml-1 (r = 0.999 9), 1.51-502.56μg · ml-1 (r = 0.999 9 ), 4.11-65.76μg · ml-1 (r = 0.999 1). The average recoveries were 93.6%, 91.7% and 92.8% respectively. The RSDs were 2.5%, 3.0% and 5.7%, respectively. Conclusion: The method is accurate and reliable and is suitable for the determination of the three organic solvents residues in sulpiride.