顶空气相色谱法测定洛伐他汀原料药中的有机溶剂残留量

目的:建立测定洛伐他汀原料药中乙醇、丙酮、乙酸乙酯、甲苯4种有机溶剂残留量的方法。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,检测器为氢火焰离子化检测器,检测器温度为280℃,进样口温度为160℃。结果:乙醇、丙酮、乙酸乙酯、甲苯的检测浓度的线性范围分别为10.0～250(r=1.0000)、10.0～250(r=0.9999)、10.0～250(r=0.9999)、1.78～89μg.mL-(1r=0.9997);平均回收率为97.6～99.1(RSD=0.9～1.9),定量限为0.22～5.61μg.mL-1;4批样品中4种有机溶剂残留量均符合《中国药典》2005年版要求。结论:该方法操作简便、精密度好,结果准确、可靠。

Determination of Residual Organic Solvents in Lovastatin by Headspace Gas Chromatography

OBJECTIVE： To establish a method for the content determination of residual organic solvents in lovastatin, i.e. alcohol, acetone, ethyl acetate and methylbenzene. METHODS： Headspace GC was adopted. The determination were separated on DB-624 capillary column using temperature programming. FID was used as detector with a temperature of 280 ℃, and the inlet temperature was 160 ℃. RESULTS： The linear ranges of alcohol, acetone, ethyl acetate and methylbenzene were 10.0-250 μg·mL^-1 （r=l.000 0）, 10.0-250μg.mL^-1 （r=0.999 9）, 10.0-250 μg·mL^-1 （r=0.999 9）, 1.78-89μg·mL^-1 （r=0.999 7）, respectively. The average recoveries ranged from 97.6% to 99.1% with RSD of 0.9%-1.9%. The determination limits were 0.22- 5.61 μg·mL^-1. The residual levels for the 4 organic solvents in 4 batches of samples were all up to the standard stipulated in Chinese Pharmacopeia （2005 edition）. CONCLUSION： The method is simple, precise, accurate and reliable.