目的 建立氣相色譜法（GC）測定高哌嗪中雜質(zhì)殘留乙二胺和哌嗪。方法 采用GC法，色譜柱為CP-sil8 CB（30 m× 0.25 mm×0.50 μm）；進樣口溫度240℃；升溫程序：60℃保持1 min，以5℃/min的速率升溫至110℃，再以40℃/min的速率升溫至200℃，保持3 min；檢測器為氫火焰離子化檢測器（FID），檢測器溫度為250℃；載氣為氮氣；分流比為2∶ 1；進樣方式為直接進樣，進樣量1 μL；體積流量：1 mL/min。結(jié)果 高哌嗪中乙二胺雜質(zhì)和哌嗪雜質(zhì)與主成分間均能有效分離，線性范圍分別為20.2～161.7 μg/mL（r=0.999 8），20.4～163.6 μg/mL（r=0.999 9）。重復(fù)性和精密度的RSD值均在規(guī)定范圍內(nèi)。結(jié)論 該方法適用于高哌嗪中乙二胺和哌嗪雜質(zhì)的準確測定和質(zhì)量控制。

Objective A GC method was established to determine the residual impurities of ethylenediamine and piperazine in homopiperazine. Methods Gas chromatography was applied to this study. The determination was carried out on CP-sil8 CB(30 m× 0.25 mm×0.50 μm). Injection temperature was 240℃. Temperature rise procedure was kept at 60℃ for 1 min, then the temperature was raised to 110℃ at the rate of 5℃/min. And the temperature was raised to 200℃ at the rate of 40℃/min for 3 min. The detector was FID, and the detector temperature was 250℃. The carrier gas was nitrogen, the split ratio was 2:1. The injection volume was 1 μL, the flow rate was 1 mL/min. Results Ethylenediamine impurity and piperazine impurity in homopiperazine can be separated from the principal component effectively. The linear range was 20.2-161.7 μg/mL (r=0.999 8), and 20.4-163.6 μg/ mL (r=0.999 9), respectively. The RSD values of repeatability and precision were within the specified range. Conclusion The method is simple, accurate and reliable, and has good specificity, and can be used for quality control of homopiperazine.

R927.2