顶空-气相色谱法测定依克多因原料中11种残留溶剂

Determination of 11 residual solvents in Ectoine raw materials by HS-GC

建立了顶空-气相色谱法同时测定依克多因中甲醇、乙醇、异丙醇、乙腈、二氯甲烷、氯仿、乙酸乙酯、乙醚、甲基叔丁基醚、甲苯、丙酮11种残留溶剂的检测方法。方法采用顶空-气相色谱法,色谱柱为Agilent DB-624毛细管柱(30 m×0.32 mm,1.8μm),检测器为氢火焰离子化检测器,进样口温度为230℃,分流进样,分流比为20:1;顶空平衡温度为80℃,平衡时间为20 min。检出成分经气相色谱质谱联用仪确认。结果显示,11种残留溶剂在所建立的色谱条件下均可以完全分离,线性关系良好,相关系数均大于0.999,精密度及回收率结果良好,该方法灵敏、高效、准确,适用于依克多因中溶剂残留的检测和质量控制。

A HS-GC method was developed for the simultaneous determination of 11 residual solvents in ectoine,including methanol,ethanol,isopropyl alcohol,acetonitrile,dichloromethane,chloroform,ethyl acetate,ether,methyl tert-butyl ether,toluene and acetone.The headspace-gas chromatography was performed on Agilent DB-624 capillary column(30 m×0.32 mm,1.8μm)with hydrogen flame ionization detector as the detector.The inlet temperature was set at 230℃andthespiltratiowas20:1.Theheadspace equilibrium temperature was 80 C with the equilibrium time 20 min.Detected components were confirmed by gas chromatographymass spectrometry.Results show that 11 residual solvents can be completely separated under the established chromatographic conditions.The linear relationships of 11 solvents are good with the correlation coefficient greater than 0.999,also the precision and recovery results are good.This method is sensitive,efficient and accurate,and also suitable for the detection and quality control of solvent residues in ectoine.