气相色谱-质谱联用技术测定虫草类口服液中甘露醇的含量

摘要

建立了气相色谱-质谱联用技术测定虫草类口服液中甘露醇含量的新方法。样品用超纯水溶解,超声提取30min,处理液经减压蒸馏至干,加入无水乙酸酐进行衍生化,最后用丙酮进行萃取,用 DB-5MS 色谱柱进行分离,提取特征离子115定量,特征离子103、85定性,外标法定量。柱温为200℃,进样口温度为180℃,氮气流速为1.0mL/min。甘露醇在5~100mg/L 范围内成线性响应关系,检出限为1mg/L,相关系数>0.99,方法相对标准偏差(n=6)为1.24%~4.35%。平均回收率在88.96%~98.36%之间。该方法前处理操作简便、样品分离效果好、成本低、回收率高、重现性好,适用于口服液中甘露醇含量的检测。%The samples were dissolved in ultrapure water and extracted by ultrasonic extractio for 30 min.The processing fluids were dried by distillation in vacuum,and derived in anhydrous acetic anhydride and then extracted with aceton,and separated by DB-5 column.Quantification analysis was performed by the external standard method,the quantitative ion was 1 15,the qualitative ions were 103 and 85.The temperature of column and injection were 200℃ and 180℃.The flow rate of nitrogen was 1.0 mL/min. The calibration curves were linear in the range of 5-100mg/L.The correlation coefficients (r)was larger than 0.99.The detection limit was 1mg/L.The average recoveries were 88.96%-98.36% with relative standard deviations (RSD,n=6)of 1.24%-4.35%.