来曲唑中残留溶剂四氯化碳顶空μ-ECD检测方法的建立和验证

Determination of Tetrachloromethane in Letrozol by Headspace Analysis with μ-ECD

摘要: 目的建立用气相色谱外标法分析来曲唑中残留溶剂四氯化碳的方法。方法采用SE-30色谱柱，50 ℃~150 ℃程序升温，微电子捕获检测器检测。结果四氯化碳能与其他组分很好的分离，分离度(α)>2.0，且峰型对称。四氯化碳浓度在0.000 516~0.020 64 μg·mL^-1内，r=0.999 9，呈现良好的线性关系，检测限为0.01 μg·g^-1。采用的顶空进样的样品处理方法回收率高且对色谱柱及检测器的污染小。结论测定方法操作简便、快速、准确性高、重复性好，可作为本品的质量控制方法。

Abstract: OBJECTIVE To establish a method for the quantitative determination of tetrachloromethane in Letrozol by GC. METHODS Tetrachloromethane was analyzed by Gas Chromatography with SE-30 column, μ-ECD detector, and programming temperature from 50 ℃ to 150 ℃. RESULTS Experimental results showed that a good separation of tetrachloromethane with other contents of sample was achieved on SE-30 column, and the separation degree was more than 2.0. The calibration curves of solvent was linear in 0.000 516-0.020 64 μg·mL^-1. The limit of detection was 0.01 μg·g^-1. CONCLUSION This method is simple, rapid, accurate and precise, and can be used for the quality control of residual tetrachloromethane in Letrozol.