University of Pardubice, Department of Analytical Chemistry, Faculty of Chemical Technology, Studentská 573, CZ-532 10 Pardubice, Czech Republic.
Talanta. 2012 Sep 15;99:316-22. doi: 10.1016/j.talanta.2012.05.058. Epub 2012 Jun 12.
A method for focused ultrasonic extraction of nitroglycerin, triphenyl amine and acetyl tributyl citrate presented in double-base propellant samples following by the gas chromatography/mass spectrometry analysis was developed. A face-centered central composite design of the experiments and response surface modeling was used for optimization of the time, amplitude and sample amount. The dichloromethane was used as the extractant solvent. The optimal extraction conditions with respect to the maximum yield of the lowest abundant compound triphenyl amine were found at the 20 min extraction time, 35% amplitude of ultrasonic waves and 2.5 g of the propellant sample. The results obtained under optimal conditions were compared with the results achieved with validated Soxhlet extraction method, which is typically used for isolation and pre-concentration of compounds from the samples of explosives. The extraction yields for acetyl tributyl citrate using both extraction methods were comparable; however, the yield of ultrasonic extraction of nitroglycerin and triphenyl amine was lower than using Soxhlet extraction. The possible sources of different extraction yields are estimated and discussed.
建立了一种针对双基推进剂样品中硝化甘油、三苯基胺和乙酰三丁基柠檬酸的聚焦超声提取方法,并用气相色谱/质谱法进行分析。实验采用中心复合面设计和响应面建模进行优化,选择时间、振幅和样品量为优化变量。二氯甲烷被用作萃取溶剂。在提取时间为 20 分钟、超声波振幅为 35%和推进剂样品量为 2.5 克的条件下,可获得最低丰度化合物三苯基胺的最大产率。最佳条件下的结果与通常用于从爆炸物样品中分离和预浓缩化合物的验证索氏提取方法的结果进行了比较。两种提取方法对乙酰三丁基柠檬酸的提取产率相当;然而,超声提取硝化甘油和三苯基胺的产率低于索氏提取。对不同提取产率的可能来源进行了估计和讨论。