GC测定奈拉滨中有机溶剂残留量

Determination of Residual Organic Solvents in Nelarabine by GC

目的建立奈拉滨中有机溶剂残留量的气相色谱分析方法。方法色谱柱为SE-54石英毛细管柱(30 m×0.53 mm,1.0μm),氢火焰离子化检测器(FID),载气为氮气,流速40 mL.min 1。进样口温度:200℃,检测器温度:250℃,分流比为50∶1,柱温为程序升温:初始温度40℃保持5 min,以50℃.min 1升至200℃保持5 min。外标法进行定量,并对分离条件进行了研究。结果甲醇、乙腈、二氯甲烷、乙酸乙酯的线性范围分别为14.93～746.4 ng(r=0.999 4),1.950～97.45 ng(r=0.999 8),2.980～149.0 ng(r=0.999 6),25.12～1 256 ng(r=0.999 8);平均回收率(n=9)分别为100.6%(RSD=1.87%),101.0%(RSD=2.27%),99.7%(RSD=3.41%),100.4%(RSD=1.52%)。结论该方法快速、准确、灵敏度高、重复性好,可作为奈拉滨中有机溶剂残留量的测定方法。

OBJECTIVE To establish a method for the determination of residual organic solvents in nelarabine by gas chromatography.METHODS Chromatographic column was capillary column SE-54（30 m×0.53 mm,1.0 μm）,with FID detector and nitrogen as carrier gas,the flow rate was 40 mL·min-1.Injector temperature was 200 ℃ and the detector temperature was 250℃,the split ratio was 50∶1,column temperature was programmed and initial temperature was 40 ℃,maintained for 5 min,raised to 200 ℃ with a rate of 50 ℃·min-1,maintained for 5 min.The external standard method was used for quantitative analysis.Analytical conditions were studied.RESULTS The standard curves were linear in the range of 14.93？746.4 ng（r =0.999 4） for methanol,1.950-97.45 ng（r=0.999 8） for acetonitrile,2.980-149.0 ng（r=0.999 6） for methylene chloride and 25.12-1 256 ng（r=0.999 8） for ethyl acetate.The average recoveries（n=9） were 100.6%（RSD=1.87%）,101.0%（RSD=2.27%）,99.7%（RSD=3.41%）,100.4%（RSD=1.52%）.CONCLUSION The method is rapid,accurate,sensitive,reproducible and can be used for detecting residual organic solvents in nelarabine.