论文部分内容阅读
目的建立测定格拉司琼中甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃残留有机溶剂含量的顶空气相色谱法。方法采用顶空气相色谱法,FID检测器,以二甲基亚砜为溶媒,顶空预热温度为95℃,预热时间为25min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-624交联毛细管柱(30m×0.53mm.i.d,3μm),采用程序升温,实现了各组分的基线分离。结果甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃在各自对应的浓度范围内,线性关系良好;甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃的最小检测限分别为0.01μg/mL、0.19μg/mL、0.02μg/mL、0.18μg/mL、0.02μg/mL、0.003μg/mL;加样回收率均在95%以上,精密度良好。结论经方法学验证,该方法灵敏、准确、可靠,可适用于格拉司琼中甲醇、乙醇、二氯甲烷、异丙醇、乙酸乙酯、四氢呋喃残留有机溶剂的测定。
OBJECTIVE To establish a headspace gas chromatographic method for the determination of residual organic solvents such as methanol, ethanol, methylene chloride, isopropanol, ethyl acetate and tetrahydrofuran in granisetron. Methods Headspace gas chromatography, FID detector, dimethylsulfoxide as solvent, the headspace preheating temperature was 95 ℃, preheating time was 25min, the inlet temperature was 180 ℃, the detector temperature was 250 ℃ , Using nitrogen as the carrier gas, using DB-624 cross-linked capillary column (30m × 0.53mm.id, 3μm), using the program temperature, to achieve the baseline separation of each component. The results showed that methanol, ethanol, dichloromethane, isopropanol, ethyl acetate and tetrahydrofuran had a good linear relationship in the corresponding concentration range. The minimum detection of methanol, ethanol, methylene chloride, isopropanol, ethyl acetate and tetrahydrofuran The limits of detection were 0.01μg / mL, 0.19μg / mL, 0.02μg / mL, 0.18μg / mL, 0.02μg / mL and 0.003μg / mL, respectively. The recoveries were above 95% with good precision. Conclusion The method is sensitive, accurate and reliable and can be applied to the determination of residual organic solvents such as methanol, ethanol, methylene chloride, isopropanol, ethyl acetate and tetrahydrofuran in granisetron.