毛细管气相色谱法测定丹参素冰片酯中有机溶剂残留

Capillary GC Method for Determining Residual Organic Solvents in Tanshinol Borneol Ester

目的建立测定丹参素冰片酯中有机溶剂残留量的毛细管气相色谱法。方法采用顶空毛细管气相色谱法,N,N-二甲基甲酰胺为溶剂,DB-WAX毛细管柱(30.0 m×0.25 mm×0.25μm),氮气为载气,FID检测器。结果乙醚、丙酮、四氢呋喃、乙酸乙酯、甲醇和乙醇6种有机溶剂均达到了完全分离,在考察的质量浓度范围内具有良好线性关系,最低检测限分别为6.48,5.33,4.79,7.43,12.87,4.81 ng,高、中、低3种质量浓度的回收率均大于98%。结论该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于丹参素冰片酯中6种残留溶剂的检测和分析。

Objective To develop a headspace capillary GC method for simultaneously determining the residual organic solvents in tanshinol borneol ester. Methods The headspace capillary GC method was adopted with N,N- dimethylformamide as the solvent. N2 was used as the carrier gas. The organic solvents were separated on the DB- WAX capillary column（ 30. 0 m × 0. 25 mm × 0. 25 μm） with FID detector. Results The six kinds of residual organic solvents ether, acetone, tetrahydrofuran, ethyl acetate, methanol and ethanol were completely separated an showed a good linearity during the investigated concentration range. Their lowest limit of detection in turn were6. 48, 5. 33, 4. 79, 7. 43, 12. 87, 4. 81 ng, respectively. The average recovery rates of high, middle and low concentrations were all more than 98%. Conclusion The accuracy and sensitivity of this method all reach the detection requirement of residual organic solvents,which can be used for detecting and analyzing 6 kinds of residual organic solvents in tanshinol borneol ester.