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
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1. 昆明医科大学,云南昆明 650500;2. 昆明制药集团股份有限公司,云南昆明 650100

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R284.1

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Simultaneous Determination of 5 Residual Solvents in Scutellarin by Head-space Gas Chromatography
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1. Kunming Medical University, Kunming 650500, China; 2. Kunming Pharmaceutical CORP., Kunming 650100, China

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    摘要:

    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-1301毛细管柱(30m×0.32mm×1.0μm),以N2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0.875,1.338,1.132,1.528,10.56μg/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。

    Abstract:

    Objective To establish a method for the determination of five residual solvents in scutellarin. Methods Head-space gas chromatography was established, the chromatographic column was DB-1301(30m×0.32mm×1.0μm), the carrier 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, 10.56μg·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.

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