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 pioneeredin showing that 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 ass 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.
An HPLC-DAD-MS method is described to analyze textile dyes in different dye classes (reactive, basic, acid, direct, disperse). The described method is sensitive enough to analyze single fibers with a length of a few millimeters or less, which makes it suitable for forensic analyses. The current paper describes the information content of the acquired data as well as the results of a validation study, in which the repeatability, specificity, and limit of detection of the method were assessed by repeated measurements of nine different dyes in the mentioned dye classes. The mass accuracy (deviation generally <2 ppm) and absorbance spectra were found to be highly stable in several measurements over a period of 8 weeks. Deviation in retention times were observed and attributed to small experimental effects and a precolumn blockage. The results show that dye analysis is possible for most fibers with a minimum length of one or a few millimeters.
The analysis of amino acids present in fingerprints has been studied several times. In this paper, we report a method for the analysis of amino acids using an fluorenylmethyloxycarbonyl chloride-derivatization for LC separation and MS detection. We have obtained good results with regard to the calibration curves and the limit of detection and LOQ for the target compounds. The extraction of the amino acids from the substrates used proved to be very efficient. Analysis of the derivatized amino acids enabled us to obtain full amino acid profiles for 20 donors. The intervariability is as expected rather large, with serine as the most abundant constituent, and when examining the total profile of the amino acids per donor, a characteristic pattern can be observed. Some amino acids were not detected in some donors, or fell out of the range of the calibration curve, where others showed a surprisingly high amount of material in the deposition analyses. Further investigations will have to address the intravariability of the amino acid profiles of the fingerprints from donors. By the development of the analytical method and the application to the analysis of fingerprints, we were able to gain insight in the variability of the constituents of fingerprints between the donors.
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