论文部分内容阅读
目的:建立气相色谱法测定高乌甲素传递体中有机溶剂戏留量的方法方法:采用FID检测器,色谱枉为DB-624(30m×0.32 mm,1.8μm),进样口及检测器温度均为250℃,载气为氮气,柱温采用程序升温:初始温度为40℃,保持10min,以8℃·min~(-1)升至120℃,保持4 min,再以40℃·min~(-1)升至200℃,保持2 min;流速为1.0 ml·min~(-1)。顶空瓶平衡温度120℃,平衡时间15 min,分流比为10:1,以二甲基亚砜为溶剂结果:在甲醇、乙醇、三氮甲烷三种溶剂均能得到良好的分离,空白对照无干扰;各自检测浓度在所考察的范围内与峰面积具有良好的线性;平均回收率为96.6%～102.7%,精密度试验及准确度试验的RSD均小于2.0%;甲醇、乙醇、三氯甲烷的最低检测限分别为20,18,9.8μg·ml~(-1)。结论:本方法简便、准确,灵敏度高,适用于高乌甲素传递体原料药中有机溶剂残留量的检测。
OBJECTIVE: To establish a gas chromatographic method for the determination of organic solvents in the lappaconitine transporter.Methods: The FID detector was used to determine the amount of organic solvent in the laporodipine transporter. The chromatographic parameters were DB-624 (30m × 0.32 mm, 1.8μm) The temperature was 250 ℃ and the carrier gas was nitrogen. The temperature of the column was raised by programmed temperature: the initial temperature was 40 ℃, kept at 10 ℃ for 8 min, then kept at 120 ℃ for 4 min and then at 40 ℃ min ~ (-1) to 200 ℃ for 2 min, and the flow rate was 1.0 ml · min ~ (-1). The equilibrium temperature of the headspace bottle was 120 ℃, the equilibration time was 15 min, the split ratio was 10: 1, and dimethylsulfoxide was used as the solvent. The results showed that methanol, ethanol and trimethylamine could be well separated in three solvents. Non-interference; the detection concentration in the range of the investigated area and the peak area has a good linearity; the average recovery was 96.6% ~ 102.7%, precision test and accuracy test RSD were less than 2.0%; methanol, ethanol, The detection limits of methane were 20, 18 and 9.8 μg · ml -1, respectively. Conclusion: The method is simple, accurate and sensitive. It is suitable for the determination of residual organic solvents in lappaconitine mediator.