静态顶空进样-气相色谱法测定维生素C含片中乙醇溶剂残留

Determination of ethanol solvent residue in vitamin C buccal tablets by static headspace injection-gas chromatography

目的采用静态顶空进样装置,建立维生素C含片中乙醇溶剂残留量的气相色谱检测方法。方法超纯水为溶剂超声提取维生素C中的溶剂残留,静态顶空进样Wax极性毛细管柱分离后氢火焰离子化检测器(FID)测定乙醇溶剂残留的含量。结果乙醇溶剂残留量与气相色谱峰面积成正比,校正曲线线性范围0.005%~0.240%;检出限0.0015%;样品加标回收率91.7%~116.2%,相对标准偏差3.4%(n=7)。结论顶空自动进样-气相色谱检测乙醇溶剂残留具有专属性好,灵敏度高,线性范围宽,准确度和精密度好的优点,适用于维生素C含片中乙醇溶剂残留的检测。

Objective To establish a method for determination of residual alcohol solvent in vitamin C buccal tablets by static headspace injection-gas chromatography.Methods After being extracted by ultrasonic extraction with ultra-pure water as solvent,the ethanol solvent residual was determined by hydrogen flame detector(FID)followed by separation by wax polar capillary column via static headspace injection.Results The ethanol solvent residual was proportional to the peak area of gas chromatography,and the linear range of the calibration curve was between 0.005%-0.240%.The detection limit was 0.0015%.The recovery of spiked samples was between 91.7%-116.2%,and the relative standard deviation was 3.4%(n=7).Conclusion The method for determination of ethanol solvent residue by headspace automatic injection-gas chromatography exhibits the advantages of good specificity,high sensitivity,wide linear range,favorable accuracy and precision,which is suitable for the detection of ethanol solvent residues in vitamin C buccal tablets.