毛细管气相色谱法测定拉米夫定中有机溶剂的残留量

Determination of Residual Organic Solvents in Lamivudine by Capillary Gas Chromatography

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。

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.