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机构地区:[1]司法部司法鉴定科学技术研究所上海市法医学重点实验室上海市司法鉴定专业技术服务平台,200063
出 处:《中国司法鉴定》2017年第3期36-39,共4页Chinese Journal of Forensic Sciences
基 金:"十三五"国家重点研发项目(2016YFC0800704);国家自然科学基金项目(81501633);上海市青年科技英才扬帆计划项目(14YF1408300);科研院所社会公益研究专项(GY2014Z-4;GY2015G-3);上海市法医学重点实验室项目(17DZ2273200);上海市司法鉴定专业技术服务平台资助项目(16DZ2290900)
摘 要:目的建立α-溴代苯丙酮的GC/MS定性方法和HPLC定量方法。方法通过参数选择和条件优化建立了α-溴代苯丙酮的GC/MS、HPLC分析方法。GC/MS方法通过程序升温对α-溴代苯丙酮进行分离分析,以特征碎片离子m/z 51,77,105进行定性分析;HPLC方法在210 nm条件下,采取恒流方式对α-溴代苯丙酮进行定量分析。结果α-溴代苯丙酮在0.2~500μg/m L的浓度范围内具有良好的线性关系,线性相关系数r大于0.995;检出限为0.1μg/m L(S/N=3);定量限为0.2μg/m L(S/N=10);方法的日间及日内精密度(RSD)均小于10%,准确度为89.3%~108.7%。结论本方法具有操作简单、灵敏度高和重现性好等优点,可应用于司法鉴定实践中α-溴代苯丙酮的定性定量分析。Objective To establish a GC/MS method and a HPLC method for the determination of α-Bromopropiophenone. Method The optimal parameters for α-Bromopropiophenone analysis were developed with GC/MS and HPLC. The separation of α-Bromopropiophenone by GC/MS was carried out by the temperature-programmed method. The characteristic fragment ions were m/z 51, 77, 105. The UV detection wavelength of HPLC method was 210nm. Results The linearity of α- Bromopropiophenone in the range from 0.2 to 500 μg/mL was good, (R〉0.995). The quantification limit of the method was 0.2 μg/mL. The inter-day and intra-day relative standard deviations (RSD) were less than 10%. Conclusion The methods developed are simple, sensitive and reproducible with their successful application in the qualitative and quantitative analysis of α-Bromopropiophenone.
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