气相色谱法测定α-酮苯丙氨酸钙中有机溶剂残留量

Determination of Residual Solvents in α-Ketophenylalanine Calcium by Gas Chromatography

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 develop a method for the determination of residual solvents in a-ketophenylalanine calcium by capillary gas chromatography. Methods： The residual solvents were separated on a DB -624 （30 m x 0.32 ram, 0.25 μm） capillary chromato- graphic column with temperature programming. The column temperature was maintained at 40℃ for 1 rain, and then raised to 180℃ at a rate of 10℃· min -1 and maintained for 2 min. N3 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 a-ketoleucine calcium were detected using an external standard method. Results： The four solvents were separated completely. There was a good hnear 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 rapid, simple, accurate and sensitive, and can be used in the determination of residual solvents in a-ketophenylalanine calcium.