Xu Xiaoma, van de Craats Anick M, Kok Eric M, de Bruyn Peter C A M
Department of Chemistry, Netherlands Forensic Institute, P.O. Box 3110, 2280 GC Rijswijk, The Netherlands.
J Forensic Sci. 2004 Nov;49(6):1230-6.
An HPLC-APCI-MS(/MS) method for the (trace) analysis of the most commonly encountered peroxide explosives, hexamethylenetriperoxidediamine (HMTD) and triacetonetriperoxide (TATP), has been developed. With this method, HMTD and TATP have been analyzed in the same run. (Pseudo-)molecular ions of these peroxides have been obtained as base peak under the same condition. A series of product ions was produced from these pseudo-molecular ions ([HMTD - 1]+ and [TATP + NH4]+) in the MS/MS analysis. We also pioneered in showing that a TATP molecular ion [TATP + H]+ can be observed with HPLC-MS/MS. The limit of detection for HMTD and TATP was 0.26 and 3.3 ng, respectively, on column by HPLC-MS in the Full Scan mode and 0.08 and 0.8, respectively, by HPLC-APCI-MS/MS in Selected Reaction Monitoring (single mass unit) mode. The method presented has been applied successfully for the identification of peroxides in the bulk solid state (powder sample), as well as in post-blast extracts originating from a forensic case. For the post-blast extracts, the use of tandem MS has been shown clearly to be of crucial importance for the identification and detection of the peroxide explosives.
已开发出一种用于（痕量）分析最常见的过氧化物炸药——六亚甲基三过氧化二胺（HMTD）和三丙酮三过氧化酮（TATP）的高效液相色谱-大气压化学电离质谱（/质谱）方法。采用该方法，可在同一次运行中对HMTD和TATP进行分析。在相同条件下，这些过氧化物的（准）分子离子作为基峰获得。在串联质谱分析中，从这些准分子离子（[HMTD - 1]+和[TATP + NH4]+）产生了一系列产物离子。我们还率先表明，通过高效液相色谱-串联质谱可以观察到TATP分子离子[TATP + H]+。在全扫描模式下，通过高效液相色谱-质谱对柱上HMTD和TATP的检测限分别为0.26 ng和3.3 ng，而在选择反应监测（单质量单位）模式下，通过高效液相色谱-大气压化学电离质谱/质谱的检测限分别为0.08 ng和0.8 ng。所提出的方法已成功应用于鉴定散装固态（粉末样品）中的过氧化物，以及源自一个法医案件的爆炸后提取物中的过氧化物。对于爆炸后提取物，串联质谱的使用已清楚表明对于过氧化物炸药的鉴定和检测至关重要。
