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目的:建立顶空气相色谱法测定洛氟普啶中有机溶剂残留量。方法:采用Agilent DB-624毛细管柱(30 m×0.32 mm,1.8μm);氮气为载气,流速为1.3 mL.min-1;分流比为1∶1;进样口温度为200℃;FID检测器,检测器温度为250℃;程序升温:初始温度40℃,保持10 min,然后以30℃.min-1升至240℃,保持5 min。顶空进样,平衡温度为100℃,平衡时间为30 min;以二甲基甲酰胺为溶剂,外标法测定洛氟普啶中甲醇、乙醇、丙酮和二氯甲烷的残留量。结果:在本文色谱条件下,甲醇、乙醇、丙酮和二氯甲烷均能得到良好的分离,空白对照无干扰,检测浓度在所考察的范围内与峰面积具有良好的线性,r=0.9993~0.9996;平均回收率为93.8%~103.6%,精密度试验及准确度试验的RSD均小于2.0%,甲醇、乙醇、丙酮和二氯甲烷检测限分别为0.765,0.948,0.463,0.680μg.mL-1。结论:本试验建立的色谱方法简便、准确,适合洛氟普啶原料中有机溶剂残留量的检测。
Objective: To establish a headspace gas chromatographic method for the determination of residual organic solvents in loofuturide. Methods: Agilent DB-624 capillary column (30 m × 0.32 mm, 1.8 μm) was used. Nitrogen was used as a carrier gas at a flow rate of 1.3 mL · min -1. The split ratio was 1: 1. The inlet temperature was 200 ℃. Detector, detector temperature was 250 ℃; temperature programmed: the initial temperature of 40 ℃, for 10 min, then 30 ℃. Min-1 rose to 240 ℃, for 5 min. Headspace injection, the equilibrium temperature was 100 ℃, the equilibration time was 30 min; with dimethylformamide as solvent, external standard method for the determination of loofopud methanol, ethanol, acetone and dichloromethane residues. Results: Under the chromatographic conditions, methanol, ethanol, acetone and dichloromethane were well separated without any interference. The detection concentration was linear with the peak area in the investigated range, r = 0.9993 ~ 0.9996 ; The average recoveries ranged from 93.8% to 103.6%. The RSDs of precision and accuracy tests were less than 2.0%. The detection limits of methanol, ethanol, acetone and dichloromethane were 0.765, 0.948, 0.463 and 0.680 μg · mL-1, respectively . Conclusion: The chromatographic method established in this study is simple and accurate, suitable for the detection of residual organic solvents in loofuturide raw materials.