摘要
建立顶空气相色谱法,同时测定雌二醇中的残留溶剂甲醇和乙醇.采用以6％氰丙基和94％二甲基聚硅氧烷为固定相的毛细管柱作为色谱柱,用氢火焰离子化检测器检测.方法学验证结果表明:甲醇质量浓度为2.01～20.1 μg/mL时残留溶剂线性关系良好(r=0.999 8),乙醇质量浓度为2.00～24.0 μg/mL时残留溶剂线性关系良好(r=0.999 8);甲醇回收率分别为106.9％、102.2％、100.8％,乙醇回收率为104.3％、103.8％、105.9％.该方法专属性强、灵敏度高、准确性好,可用于雌二醇中残留溶剂的测定.
Abstract
The paper established a headspace gas chromatography method and simultaneously determined the residual solvents methanol and ethanol in estradiol.The paper uses a capillary column with 6％cyanopropyl and 94％dimethylpolysiloxane as stationary phases as the chromatographic column,and is detected by a hydrogen flame ionization detector.The methodological validation results indicate that methanol ranges from 2.01 to 20.1 μ.The linear relationship is good within the range of g/mL(r=0.999 8),and ethanol ranges from 2.00 to 24.0 µ.The linear relationship is good within the range of g/mL(r=0.999 8);The recovery rates of methanol are 106.9％,102.2％,and 100.8％,respectively,while the recovery rates of ethanol are 104.3％,103.8％,and 105.9％.This method has strong specificity,high sensitivity,and good accuracy,and can be used for the determination of residual solvents in estradiol.
维普
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