摘要
目的:建立测定α-酮缬氨酸钙原料药中有机溶剂乙醇、乙醚、丙酮、乙酸乙酯残留量的方法。方法:采用顶空气相色谱法。色谱柱为DB-624石英毛细管柱,柱温采用程序升温,氢火焰离子化检测器,检测器温度为250℃,进样口温度为150℃,以水为溶剂。结果:乙醇、乙醚、丙酮、乙酸乙酯检测浓度的线性范围均为0.01～2.0mg·mL-(1r均为0.9999);平均回收率为98.6%～99.7%(RSD=1.0%～1.5%);定量限为0.51～5.04μg·mL-1;3批样品中4种有机溶剂残留量均符合《中国药典》要求。结论:本方法简单、准确、灵敏度高、重复性好,可用于该药物中有机溶剂残留量的测定。
OBJECTIVE： To establish a method for the content determination of residual organic solvents in α-ketovaline calcium, such as alcohol, ethyl ether, acetone, and ethyl acetate. METHODS： Headspace gas chromatography was adopted. Residual organic solvents were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 250 ℃, the inlet temperature was 150 ℃ with water as the solvent. RESULTS： The linear ranges of alcohol, ethyl ether, acetone and ethyl acetate all were 0.01～2.0 mg·mL-1 （r=0.999 9）. The average recoveries were 98.6%～99.7% （RSD=1.0%～1.5%）.The determination limits were 0.51～5.04 μg·mL-1. The residual levels of 4 kinds of organic solvents in 3 batches of samples were all up to the standard stated in Chinese Pharmacopeia. CONCLUSION： The method is simple, accurate, sensitive and reproducible. It can be used for the determination of the residual organic solvents in α-ketovaline calcium.
出处
《中国药房》
CAS
CSCD
北大核心
2011年第5期451-452,共2页
China Pharmacy
