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目的:建立格列吡嗪中的残留溶剂丙酮、四氢呋喃、甲醇的分离测定方法。方法:采用 Agilent-INNOWAX 石英毛细管气相色谱柱(30 m×0.32 mm,0.25 μm),载气为氮气,氧火焰离子化柃测器,进样口温度为200℃,检测器温度为250℃。柱温采用程序升温:初始温度为40℃,维持8 min,以100℃·min~(-1)速率升至180℃,维持8 min;流速为1 mL·min~(-1)。以0.5mol·L~(-1)氢氰化钠溶液为样品的溶剂。结果:丙酮、四氢呋喃、甲醇的检测限分别为0.025,0.021,0.716 μg·mL~(-1);定量限分别为0.396,0.133,3.600 μg·mL~(-1);平均回收率(n=9)分别为93.1%,89.6%,91.7%。结论:本法操作简便,灵敏度高、准确性强,适用于格列吡嗪中残留溶剂的检测。
Objective: To establish a method for the separation and determination of residual solvents acetone, tetrahydrofuran and methanol in glipizide. Methods: The Agilent-INNOWAX quartz capillary column (30 m × 0.32 mm, 0.25 μm) was used. The carrier gas was nitrogen and oxygen flame ionization detector. The inlet temperature was 200 ℃ and the detector temperature was 250 ℃. The temperature of the column was programmed as follows: the initial temperature was 40 ℃ and maintained at 8 ℃ for 8 min. The temperature was raised to 180 ℃ at 100 ℃ · min ~ (-1) for 8 min. The flow rate was 1 mL · min ~ (-1). A 0.5 mol·L -1 sodium hydocyanate solution was used as the sample solvent. Results: The detection limits of acetone, tetrahydrofuran and methanol were 0.025, 0.021 and 0.716 μg · mL -1, respectively. The limits of quantification were 0.396,0.133 and 3.600 μg · mL -1, respectively. The average recoveries (n = 9) were 93.1%, 89.6% and 91.7% respectively. Conclusion: This method is simple, sensitive, accurate and suitable for the determination of residual solvents in glipizide.