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顶空气相色谱法同时测定牛黄中7种残留溶剂

[Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

作者信息

Chi Shuyao, Wu Dike, Sun Jinhong, Ye Ruhan, Wang Xiaoyan

出版信息

Se Pu. 2014 May;32(5):553-7. doi: 10.3724/sp.j.1123.2014.01013.

Abstract

A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

摘要

建立了一种顶空气相色谱(HS-GC)法,用于同时测定牛黄中7种残留溶剂(石油醚(60 - 90℃)、丙酮、乙酸乙酯、甲醇、二氯甲烷、乙醇和乙酸丁酯)。采用DB-WAX毛细管柱和火焰离子化检测器(FID)对残留溶剂进行分离和检测,并采用内标法进行定量。对平衡温度和平衡时间等色谱条件进行了优化。在优化条件下,7种残留溶剂在规定浓度范围内均呈现良好的线性关系,相关系数良好(不小于0.999 3)。在3个加标水平下,7种残留溶剂的回收率为94.7% - 105.2%,相对标准偏差(RSD)小于3.5%。该方法的检测限(LOD)为0.43 - 5.23 mg/L,定量限(LOQ)为1.25 - 16.67 mg/L。该方法简便、快速、灵敏、准确,适用于同时测定牛黄中7种残留溶剂。

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