顶空气相色谱法同时测定灯盏花乙素中5种有机溶剂残留量

Simultaneous Determination of 5 Residual Solvents in Scutellarin by Head-space Gas Chromatography

目的建立灯盏花乙素中5种有机溶剂残留量的分离测定方法。方法采用顶空进样毛细管气相色谱法，色谱柱为DB一1301毛细管柱（30m：：〈0．32mmx1．0μm），以N：为载气，FID检测器，程序升温，N，N-二甲基乙酰胺（DMA）为溶解介质。结果5种有机溶剂完全分离，在所考察的浓度范围内具有良好的线性，r为0．9939-0．9999，甲醇、乙醇、丙酮、二氯甲烷、N，N-二甲基甲酰胺（DMF）的最低检测限分别为0．875，1．338，1．132，1．528，10．561,μg／mL，精密度RSD均小于2％，平均回收率为99．15％-103．32％．结论本实验建立的方法简便灵敏，结果准确可靠，可用于灯盏花乙素中有机溶剂残留量的检测。

Objective To establish a method for the determination of five residual solvents in seutellarin. Methods Head- space gas chromatography was established, the chromatographic column was DB-1301 （30mx0.32mmxl.0μm）, the c, arrier gas was N2, the detector was FID, temperature was controlled by program and the solvent was N, N-Dimethylacetamide（DMA）. Results Five residual solvents were completely separated. A good linearity （r=0.9939-0.9999）was obtained. The detection limits of methanol, ethanol, acetone, dichloromethane and DMF were 0.875, 1.338, 1.132, 1.528, 10.561μg＇mL-1 respectively;the RSDs of precision were less than 2%; the average recovery rates of the preparation were in the range of 99.15%-103.32%. Conclusion The method is simple, sensitive, accurate and can be used for the quality control of scutellarin.