GC测定奈拉滨中有机溶剂残留量

Determination of Residual Organic Solvents in Nelarabine by GC

关键词:  气相色谱法  奈拉滨  有机溶剂残留量

Key words:  GC  nelarabine  residual organic solvents

摘要:

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，1.0 μm)，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。

Abstract:

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.