目的阐述α-溴代苯丙酮的特性及其在制毒过程中的危害性,建立α-溴代苯丙酮的检验方法。方法通过选择和优化建立了α-溴代苯丙酮的FTIR、GC/MS、GC/FID分析条件。结果用FTIR和GC/MS对α-溴代苯丙酮进行定性分析,给出了α-溴代苯丙酮的质谱裂解方式。用GC/FID分析了方法的检测限、线性、精密度。在优化条件下,α-溴代苯丙酮在0.01~0.50 mg/m L的线性范围内具有良好的线性关系,线性相关系数r为0.9997;检出限为0.2μg/m L(S/N=3);0.1 mg/m Lα-溴代苯丙酮峰面积的RSD=1.59%(n=6)。结论本方法具有操作简单、灵敏度高和重现性好等优点,可应用于α-溴代苯丙酮检验鉴定。
Objective Alfa-Bromopropiophenone, often used to synthesize ephedrine, has been listed and controlled as the first category of precursor chemicals by the State since May 12, 2014. Therefore, the characteristics and hazardousness involving in ephedrine manufacturing with α-Bromopropiophenone should be studied. As such, the analysis procedure of α-Bromopropiophenone has been established in this paper. Methods The optimal parameters for α-Bromopropiophenone analysis were developed with FTIR, GC/MS and GC/FID. Results Alfa-Bromopropiophenone(tR=5.064min) presented its characteristic fragmental ion peaks at m/z 105.0(base peak), m/z 77.2 and m/z 51.2. A possible mass spectrogram of α-Bromopropiophenone was given. The infrared absorption spectra were shown in 3060, 2980, 2860, 1690, 1340, 1240, 1160, 1080, 1590, 1450, 843, 706, 542 and 646 cm-1. Under the optimal conditions, a good linearity was observed for α-Bromopropiophenone in 0.01-0.50mg/m L and the correlation coefficient was 0.9997. The LOD(S/N=3) was 0.2 μg/m L. The RSD was 1.59 % for 0.1mg/m L of α-Bromopropiophenone(n=6). Conclusion The method developed here is simple, sensitive and reproducible with its successful application into the qualitative and quantitative analysis of α-Bromopropiophenone.