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目的:建立阿魏酸哌嗪中苯、氯乙醇与吡啶等残留溶剂的测定方法。方法:采用GC法,以DB-624(30 m×0.53 mm,1.0μm)弹性石英毛细管柱为色谱柱,载气为氮气,采用氢火焰离子化检测器;起始温度为50℃,维持5 min,以10℃·min~(-1)的速率升温至80℃,再以50℃·min~(-1)的速率升温至200℃,维持4 min;进样口温度为200℃,检测器温度为220℃;分流比为1∶1;进样量为1μl;柱流速为3 ml·min~(-1)。结果:苯在0.16~0.96μg·ml~(-1)的浓度范围内线性关系良好(r=0.999 5),平均回收率为95.7%(RSD=2.1,n=9),检测限为0.16 ng;氯乙醇在16.11~96.65μg·ml~(-1)的浓度范围内线性关系良好(r=0.999 7),平均回收率为97.8%(RSD=2.1,n=9),检测限为0.62 ng;吡啶在15.87~95.23μg·ml~(-1)的浓度范围内线性关系良好(r=0.999 8),平均回收率为99.2%(RSD=1.3,n=9),检测限为0.15 ng。结论:本测定方法可靠、简便、结果准确、稳定性好,适用于本品残留溶剂的测定。
Objective: To establish a method for the determination of residual solvents such as benzene, chloroethanol and pyridine in piperazine ferulate. Methods: GC-MS was performed on a DB-624 (30 m × 0.53 mm, 1.0 μm) capillary column with a carrier gas of nitrogen gas using a flame ionization detector at an initial temperature of 50 ° C min, the temperature was raised to 80 ℃ at the rate of 10 ℃ · min ~ (-1), then the temperature was raised to 200 ℃ at the rate of 50 ℃ · min ~ (-1) for 4 min; the temperature of the inlet was 200 ℃, The temperature was 220 ℃. The split ratio was 1: 1. The injection volume was 1μl. The column flow rate was 3 ml · min ~ (-1). Results: The linear range was 0.16 ~ 0.96μg · ml ~ (r = 0.999 5). The average recovery was 95.7% (RSD = 2.1, n = 9) (R = 0.999 7), the average recovery was 97.8% (RSD = 2.1, n = 9), and the detection limit was 0.62 ng The average recovery of pyridine was 99.2% (RSD = 1.3, n = 9) and the detection limit was 0.15 ng. The average recovery of pyridine was in the range of 15.87 ~ 95.23μg · ml ~ (-1) Conclusion: The method is reliable, simple, accurate, stable and suitable for the determination of residual solvents in this product.