GC测定氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪的残留量

Determination of N-Methyl Piperazine and Piperazine in Ofloxacin and Norfloxacin by GC

关键词:  气相色谱法  N-甲基哌嗪  哌嗪  氧氟沙星  诺氟沙星

Key words:  GC  N-methyl piperazine  piperazine  ofloxacin  norfloxacin

摘要:

目的 建立气相色谱法测定氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪的残留量的方法。方法 采用Agilent HP CAM 毛细管色谱柱(30.0 m×0.25 mm，0.25 μm)；进样口温度为230 ℃；FID检测器温度为280 ℃；柱温：程序升温，70 ℃保持3 min，然后以40 ℃·min^-1的速率升温至180 ℃，保持2 min；以氮气为载气，流速为2.0 mL·min^-1；直接进样，进样量为0.2 μL；以水为溶解介质，以吡啶为内标，测定了氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪的残留量。结果 N-甲基哌嗪、哌嗪与内标均能良好分离，线性范围分别为10.09~201.88 μg·mL^-1(r=0.999 6)，10.08~201.60 μg·mL^-1(r=0.999 5)。结论 该方法重复性良好，回收率符合规定，适用于氧氟沙星和诺氟沙星中N-甲基哌嗪和哌嗪残留量的测定。

Abstract:

OBJECTIVE To establish a method for determination of N-methyl piperazine and piperazine in ofloxacin and norfloxacin. METHODS The determination was carried out with Agilent HP CAM capillary column (30.0 m×0.25 mm, 0.25 μm) and FID detector. The inlet temperature was 230 ℃ and the detector temperature was 280 ℃. The column temperature rose by program: the initial temperature was 70 ℃, maintained for 3 min, raised to 180 ℃ with a rate of 40 ℃·min^-1, maintained for 2 min, The carries gas was nitrogen and the flow rate of carries gas was 2.0 mL·min^-1, the direct injection was used and the injection volume was 0.2 μL. The dissolved medium used was water and the internal standard was pyridine. RESULTS N-methyl piperazine and piperazine could be separated from internal standard in chromatogram obtained from system suitability test. The calibration curves were linear in the range of 10.09-201.88 μg·mL^-1(r=0.999 6) for N-methyl piperazine, 10.08-201.60 μg·mL^-1(r=0.999 5) for piperazine. CONCLUSION The repeatability and recovery met requirements, it can be applied in determination of N-methyl piperazine and piperazine in ofloxacin and norfloxacin.