毛细管气相色谱法测定拉米夫定中有机溶剂的残留量

目的:建立以毛细管气相色谱法测定拉米夫定中有机溶剂残留量的方法。方法:色谱柱为DB-624石英毛细管柱,柱温采用程序升温,载气为氮气,流速为40mL.min-1,进样口温度为230℃,检测器温度为250℃,分流比为20∶1。结果:有机溶剂甲醇、乙醇、乙酸乙酯、正己烷和吡啶的检测浓度的线性范围分别为60.0～420.0(r=0.9993)、100.0～700.0(r=0.9998)、100.0～700.0(r=0.9997)、5.8～40.6(r=0.9991)、4.0～28.0μg.mL-1(r=0.9999);平均回收率为98.4%～100.1%(RSD=2.0%～3.2%);最低检出限为0.26～0.88ng;3批样品中5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、重现性好,可用于该制剂中有机溶剂残留量的测定。

Determination of Residual Organic Solvents in Lamivudine by Capillary Gas Chromatography

OBJECTIVE:To develop capillary gas chromatography method for the determination of residual organic solvents in lamivudine.METHODS:The residual organic solvents were separated on DB-624 capillary column using temperature programming.The carrier was nitrogen gas,the flow rate was 40mL·min-1,the inlet temperature was 230℃,the detector temperature was 250℃ and the split ratio was 20∶1.RESULTS:The linear ranges of methanol,ethanol,ethyl acetate,N-hexane and pyridine were 60.0～420.0(r=0.999 3),100.0～700.0(r=0.999 8),100.0～700.0(r=0.999 7),5.8～40.6(r=0.999 1)and 4.0～28.0μg·mL-1(r=0.999 9),respectively.The average recoveries were ranged from 98.4% to 100.1% with RSD ranged at 2.0% ～ 3.2%.The detection limits were 0.26～0.88ng.The residual levels for the five organic solvents in 3 batches of samples were all up to the standard stipulated in China Pharmacopeia.CONCLUSION:The method is simple,accurate,sensitive and reproducible,it can be used for the determination of the residual organic solvents in lamivudine.