摘要
目的建立顶空气相色谱法测定酮亮氨酸钙中有机溶剂残留量。方法采用DB-624（0.25μm,30 m×0.32mm）毛细管柱,程序升温。柱温为40℃,保持5 min,10℃·min-1升温至180℃,保持2 min。以氮气为载气,检测器为氢火焰离子化检测器,采用顶空进样方式。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具有良好的线性关系,r为0.995 4~0.998 1,平均回收率为100.7%~107.6%（RSD〈5.0%,n=6）。结论该方法快速、简便、准确,灵敏度好。可以用于测定酮亮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-ketoleucine calcium by headspaee gas chromatography. Methods The residual solvents were separated on DB-624 （0.25 μm, 30 m × 0.32 mm） capillary chromatographic column with temperature programming. The column temperature was maintained at 40℃ for 5 min, then raised at a rate of 10℃ · min ^-1 to 180℃ and maintained for 2 min. External standard method was used to determine methanol, ethanol, aceticether, and tetrahydrofuran in a-ketoleucine calcium. Results The 4 solvents were separated completely. There was a good linearity relationship between the peak area and the concentration of each solvent （r was 0.995 4 -- 0.998 1）. The average recovery of the 4 solvents was 100.7% -- 107.6% （ RSD 〈 5.0%, n = 6 ）. Conclusion The method is rapid, simple, accurate and sensitive, and can be used for the determination of residual solvents in a-ketoleucine calcium.
出处
《中南药学》
CAS
2015年第7期760-762,共3页
Central South Pharmacy
关键词
顶空气相色谱法
酮亮氨酸钙
残留溶剂
headspace gas chromatography
α-ketoleucine calcium
residual solvent
