色谱

色谱 ›› 2014, Vol. 32 ›› Issue (5): 553-557.DOI: 10.3724/SP.J.1123.2014.01013

• 技术与应用 • 上一篇    

顶空气相色谱法同时测定人工牛黄中7种残留溶剂

池舒耀1,2, 伍迪科1, 孙晋红1, 叶汝汉1, 王晓燕1   

  1. 1. 广州法尔麦兰药物技术有限公司, 广东 广州 510070;
    2. 中国广州分析测试中心, 广东 广州 510070
  • 收稿日期:2014-01-07 修回日期:2014-01-27 出版日期:2014-05-08 发布日期:2014-04-26
  • 通讯作者: 池舒耀
  • 基金资助:

    广东省科技计划项目（2012B040307002）.

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

CHI Shuyao1,2, WU Dike1, SUN Jinhong1, YE Ruhan1, WANG Xiaoyan1   

  1. 1. Guangzhou PharmaLab Co. Ltd., Guangzhou 510070, China;
    2. China National Analysis Centre (Guangzhou), Guangzhou 510070, China
  • Received:2014-01-07 Revised:2014-01-27 Online:2014-05-08 Published:2014-04-26

PDF

369

被引次数

18

摘要：

建立了同时测定人工牛黄中石油醚（60~90 ℃）、丙酮、乙酸乙酯、甲醇、二氯甲烷、乙醇、乙酸丁酯7种残留溶剂的顶空气相色谱分析方法。以Agilent DB-WAX毛细管色谱柱为分离柱，氢火焰离子化检测器检测，内标法定量，并考察了顶空平衡温度、加压时间、平衡时间等对残留溶剂测定的影响。在优化的条件下，7种残留溶剂在选择的浓度范围内线性关系良好，相关系数（r）均不小于0.9993；在高、中、低3个加标水平下，平均回收率为94.7%~105.2%，相对标准偏差（RSD）均不大于3.5%。方法的检出限（LOD）为0.43~5.23 mg/L，定量限（LOQ）为1.25~16.67 mg/L。该方法操作简单、准确灵敏、高效快捷，适用于人工牛黄中7种残留溶剂的同时检测。

关键词: 残留溶剂, 顶空气相色谱法, 内标法, 人工牛黄

Abstract:

A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 ℃), 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 0.9993) 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.

Key words: bovis calculus artifactus, headspace gas chromatography (HS-GC), internal standard method, residual solvent

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