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目的建立测定安立生坦原料药中可能残留的6种有机溶剂(甲醇、乙醚、二氯甲烷、乙酸乙酯、1,4-二氧六环、N,N-二甲基甲酰胺)含量的检测方法。方法采用顶空气相色谱法,色谱柱为DB-624毛细管柱(30.0 m×0.53 mm,3.00μm),氢火焰离子化检测器(FID),进样口温度250℃,检测器温度300℃;载气为高纯氮气,恒压模式,压力2 psi;柱温为升温程序,50℃保持10 min,以20℃·min-1升温升至200℃,保持4 min;顶空瓶平衡温度100℃,平衡时间30 min。结果6种残留溶剂色谱峰的理论板数均>10 000,相邻峰的分离度均>2.0,甲醇、乙醚、二氯甲烷、乙酸乙酯、1,4-二氧六环、N,N-二甲基甲酰胺的线性关系良好(r分别为0.999 6,0.999 2,0.999 5,0.999 3,0.999 3,0.999 6);精密度与重复性RSD均<5.0%;最低检出浓度分别为0.36,0.034,0.51,0.43,0.45,5.27μg·mL-1;平均回收率均在90%以上;供试品溶液24 h内稳定。结论该气相色谱法操作简便,准确,灵敏度高,可用于检测安立生坦原料药中有机溶剂的残留量。
OBJECTIVE To establish a method for the determination of 6 kinds of organic solvents (methanol, ether, methylene chloride, ethyl acetate, 1,4-dioxane, N, N-dimethylformamide) Detection method. Methods The capillary column was DB-624 capillary column (30.0 m × 0.53 mm, 3.00 μm) with flame ionization detector (FID). The inlet temperature was 250 ℃ and the detector temperature was 300 ℃. The carrier gas was high purity nitrogen, constant pressure mode, pressure 2 psi; column temperature for the temperature program, 50 ℃ for 10 min, 20 ℃ · min-1 temperature rose to 200 ℃, hold 4 min; headspace bottle balance temperature 100 ℃, balance time 30 min. Results The number of theoretical plates of the six residual solvent peaks were both> 10 000 and the resolution of adjacent peaks were both> 2.0. Methanol, diethyl ether, dichloromethane, ethyl acetate, 1,4-dioxane, N, N -dimethylformamide had good linearity (r = 0.999 6,0.999, 2,0.999 5,0.999 3,0.999 3,0.999 6 respectively). The RSDs of precision and repeatability were all less than 5.0%, and the lowest detectable concentrations were 0.36,0.034,0.51,0.43,0.45,5.27μg · mL-1; the average recovery rate was above 90%; the test solution was stable within 24 h. Conclusion The gas chromatography is simple, accurate and sensitive. It can be used to detect the residues of organic solvents in anritsyram raw material.