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目的建立直接进样气相色谱法测定卡格列净中甲醇、乙腈、乙酸乙酯、甲苯、四氢呋喃和正庚烷共6种有机溶剂的残留量。方法采用毛细管气相色谱法测定,毛细管色谱柱为CP-SIL 8CB(25 m×0.53 mm,5.0μm)柱,采用FID检测器,以氮气为载气,流速为3.0 m L·min-1,采用程序升温,初始柱温为40℃,保持6 min,以30℃·min-1升至160℃,保持2 min,再以30℃·min-1升至200℃,保持3 min,进样口温度为160℃,检测器温度为250℃,溶液直接进样,分流比为20∶1,用内标法计算6种溶剂的残留量。结果在本色谱条件下6种残留溶剂在各自浓度范围内均具有良好的线性关系,平均回收率为98.8%~107.4%(n=9),RSD为0.7%~3.9%(n=9),重复性RSD≤2.5%(n=6)。结论本方法适用于同时测定卡格列净中甲醇、乙腈、乙酸乙酯、甲苯、四氢呋喃和正庚烷共6种有机溶剂残留量。
OBJECTIVE To establish a direct injection gas chromatographic method for the determination of the residues of 6 organic solvents, including methanol, acetonitrile, ethyl acetate, toluene, tetrahydrofuran and n-heptane, in cagaprel. The method was determined by capillary gas chromatography. The capillary column was CP-SIL 8CB (25 m × 0.53 mm, 5.0 μm) column. FID detector was used with nitrogen as the carrier gas and the flow rate was 3.0 m L · min-1. The temperature was programmed and the initial column temperature was 40 ° C and maintained for 6 min. The temperature was raised to 160 ° C at 30 ° C · min-1 for 2 min and then to 200 ° C at 30 ° C · min-1 for 3 min. The temperature was 160 ° C, the detector temperature was 250 ° C, and the solution was injected directly with a split ratio of 20: 1. Six residual solvents were calculated by internal standard method. Results The results showed that there was a good linear relationship between the six residual solvents in the range of their concentration under the chromatographic conditions. The average recoveries were 98.8% -107.4% (n = 9) and RSDs were 0.7% -3.9% (n = 9) Repeatability RSD ≤ 2.5% (n = 6). Conclusion This method is suitable for the simultaneous determination of 6 residues of 6 organic solvents, including methanol, acetonitrile, ethyl acetate, toluene, tetrahydrofuran and n-heptane, in cagaprel.