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目的:建立顶空毛细管气相色谱法测定阿折地平中有机溶剂残留量的方法。方法:采用CP-624毛细管色谱柱(30m×0.32 mm,8μm);载气为氮气,进样口温度为200℃;FID检测器,检测器温度为250℃;柱温采取程序升温,起始温度55℃,保持8 min,然后以10℃·min~(-1)的升至195℃,持续10 min。顶空进样,平衡温度为90℃,平衡时间为30 min;以二甲亚砜为溶剂,测定阿折地平原料药中乙醇、乙腈、乙酸乙酯和甲苯的残留量。结果:在本文的色谱条件下,各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r=0.997 0～0.999 0,平均回收率为95.4%～98.7%。结论:本方法灵敏、准确、可靠,可用于阿折地平中残留溶剂的检测。
OBJECTIVE: To establish a method for the determination of residual organic solvents in azadiraftin by headspace capillary gas chromatography. Methods: The CP-624 capillary column (30m × 0.32 mm, 8μm) was used. The carrier gas was nitrogen and the inlet temperature was 200 ℃. The detector temperature was 250 ℃ with FID detector. The temperature was maintained at 55 ° C for 8 min and then increased to 195 ° C at 10 ° C min -1 for 10 min. Headspace sampling, the equilibrium temperature of 90 ° C, the equilibration time of 30 min; with dimethyl sulfoxide as solvent, determination of azadorphin API in ethanol, acetonitrile, ethyl acetate and toluene residues. Results: Under the chromatographic conditions, all the organic solvents could be effectively separated. The linear range was 0.997 0 ~ 0.999 0 and the average recovery was 95.4% ~ 98.7%. Conclusion: The method is sensitive, accurate and reliable and can be used for the determination of residual solvents in.