摘要
目的:建立气相色谱-质谱(GC—MS)快速测定氟乙酰胺的方法。方法:样品经乙酸乙酯提取,离心后取上清液直接进样测定,通过色谱柱的选择和条件的优化,确定最佳分析条件。结果:氟乙酰胺的保留时间为12.63min,氟乙酰胺浓度在0.05—2.00μg/ml范围的标准曲线,其线性相关系数r=1.000,样品加标回收率在92.5%~99.9%之间,相对标准偏差(脑D)为0.94%。当取样量为1g时,最低检出浓度为0.05mg/kg。结论:该方法简便、快速,减少了溶剂及样品基质对测定的干扰,方法精密度较好,准确度较高,结果较满意,可用于中毒样品中氟乙酰胺的测定。
Objective:To develop a method for determination of fluoroacetamide by gas chromatography - massspectrometry (GC- MS). Methods:Fluoroaeetamide extracted with ethyl acetate was centrifuged and the supernatant was analyzed. Results: Retention time of fluoroacetamide was 12. 63 min, calibration curve was linear( correlation coefficient r = 1. 000) within the range of 0. 05 - 200 μg/ml. The recovery range was 92. 5% - 99. 9% , the relative standard deviation (RSD) of the method 0. 94% and the limit of determination (LOD) 0. 05 mg/kg. Conclusion:The method is simple, quick and can reduce the interference from solvent and sample matrix. The method can be used to determine the fluoroacetamide in poisoning samples with satisfactory sensitivity, accuracy and precision.
出处
《中国卫生检验杂志》
CAS
2009年第2期309-310,328,共3页
Chinese Journal of Health Laboratory Technology