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目的建立毛细管气相色谱法测定褪黑素类似物AGO中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯5种有机溶剂的残留量。方法采用DB-Wax(30 m×0.45 mm,0.85μm)毛细管色谱柱;氢火焰离子化检测器(FID);程序升温:初始温度45℃(维持9 min),以30℃.min 1速率升温至200℃(维持9 min);载气为氮气,柱流速为3.5 mL.min 1;进样口温度:200℃;检测器温度:250℃;分流直接进样,二甲基亚砜为溶剂,乙腈为内标物,内标法测定残留溶剂的含量。结果各组分分离完全,在所考察的浓度范围内线性关系良好,其中乙醇、乙酸乙酯、二氯甲烷、四氢呋喃、甲苯的线性范围分别为107.44~1 074.4μg.mL 1(r=0.999 9),108.24~1 082.4μg.mL 1(r=0.999 7),18.550~185.50μg.mL 1(r=0.999 8),14.208~142.08μg.mL 1(r=0.999 4),19.074~190.74μg.mL 1(r=0.999 9),平均回收率为98%~102%。结论该方法操作简单,精密度好,准确可靠,可用于该药物有机溶剂残留量的测定。
OBJECTIVE To establish a capillary gas chromatographic method for the determination of the residues of five organic solvents, ethanol, ethyl acetate, methylene chloride, tetrahydrofuran and toluene in the melatonin AGO analogs. Methods The capillary column with DB-Wax (30 m × 0.45 mm, 0.85 μm) was used as the capillary column. The temperature was raised at 45 ℃ for 9 min and the temperature was raised at 30 ℃ .min 1 To 200 ° C for 9 min; the carrier gas was nitrogen and the column flow rate was 3.5 mL.min 1; the inlet temperature was 200 ° C; the detector temperature was 250 ° C; split direct injection and dimethyl sulfoxide as solvent , Acetonitrile as internal standard, internal standard method to determine the content of residual solvents. Results The components were completely separated and had a good linear relationship in the investigated concentration range. The linear ranges of ethanol, ethyl acetate, dichloromethane, tetrahydrofuran and toluene were 107.44 ~ 1074.4μg.mL 1 (r = 0.999 9 ), 108.24 ~ 1082.4μg.mL 1 (r = 0.999 7), 18.550 ~ 185.50μg.mL 1 (r = 0.999 8), 14.208 ~ 142.08μg.mL 1 (r = 0.999 4), 19.074 ~ 190.74μg. mL 1 (r = 0.999 9), the average recovery was 98% ~ 102%. Conclusion The method is simple, accurate, accurate and reliable, and can be used for the determination of residual amount of organic solvents in this medicine.