气相色谱法测定α-酮苯丙氨酸钙中有机溶剂残留量

摘要

To develop a method for the determination of residual solvents inα-ketophenylalanine calcium by capillary gas chromatography. Methods:The residual solvents were separated on a DB-624(30 m × 0. 32 mm, 0. 25 μm) capillary chromato-graphic column with temperature programming. The column temperature was maintained at 40℃ for 1 min,and then raised to 180℃at a rate of 10℃·min-1 and maintained for 2 min. N2 was used as the carrier gas, and FID was used as the detector with temperature of 250 ℃. The injector temperature was 200 ℃ and the split ratio was 10∶1, and direct injection was adopted. Methanol, ethanol, ethyl acetate and tetrahydrofuran in α-ketoleucine calcium were detected using an external standard method. Results:The four solvents were separated completely. There was a good linear relationship between the peak area and the concentration of each solvent ( r=0. 997 2-0. 999 5). The average recovery of the four solvents was 95. 47%-100. 26%(RSD≤4. 7%, n=9). Conclusion:The method is rap-id, simple, accurate and sensitive, and can be used in the determination of residual solvents in α-ketophenylalanine calcium.%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0.9972~0.9995)；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。