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目的:建立毛细管气相色谱法测定α-酮苯丙氨酸钙中有机溶剂残留量。方法:采用DB-624(30 m×0.32 mm,0.25μm)毛细管柱,程序升温。柱温为40℃,保持1 min,以10℃·min~-1升温至180℃,保持2 min。载气为氮气,检测器为氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃,分流比为10∶1,采用直接进样方式。外标法测定甲醇、乙醇、乙酸乙酯、四氢呋喃的量。结果:4种溶剂均有良好的分离度,在所考察的浓度范围内与峰面积均具有良好的线性(r为0.997 2~0.999 5);平均回收率为95.47%~100.26%(RSD≤4.7%,n=9)。结论:该方法快速、简便、准确,灵敏度好,可以用于测定酮苯丙氨酸钙中的有机溶剂残留量。
Objective: To establish a capillary gas chromatographic method for the determination of residual organic solvents in α-ketophenylalanine calcium. Methods: DB-624 (30 m × 0.32 mm, 0.25 μm) capillary column was used to program temperature. The column temperature was 40 ℃ for 1 min, and the temperature was raised to 180 ℃ at 10 ℃ · min ~ -1 for 2 min. The carrier gas is nitrogen, the detector is a hydrogen flame ionization detector, the inlet temperature is 200 ° C, the detector temperature is 250 ° C, the split ratio is 10: 1, and the direct injection mode is adopted. External standard method for the determination of methanol, ethanol, ethyl acetate and tetrahydrofuran. Results: All the four solvents showed good linearity (r = 0.997 2 ~ 0.999 5) and the average recoveries ranged from 95.47% to 100.26% (RSD≤4.7 %, n = 9). Conclusion: The method is rapid, simple, accurate, sensitive and can be used to determine the residual amount of organic solvents in calcium ketophenate.