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机构地区:[1]贵阳市公安局,贵阳550007 [2]公安部物证鉴定中心,北京100038
出 处:《刑事技术》2016年第1期50-53,共4页Forensic Science and Technology
基 金:公安部重点研究计划项目(201301ZDYJ007)
摘 要:目的运用钩吻HPLC指纹图谱分析方法对其不同产地来源进行数据分析。方法取钩吻药材1 g,加45 m L水,煎煮2 h,摇匀过滤,进样量10μL,色谱条件采用Welchrom C18柱,洗脱流动相:乙腈(A)-0.025%三乙胺水溶液(B),梯度洗脱(0 min,0.5%A;5 min,1%A;10 min,3%A;15 min,8%A;20 min,15%A;40 min,30%A;46 min,36%A;60 min,65%A),流速为1.0 m L/min,柱温30℃,检测波长272 nm。分别测定9批钩吻的样本图谱,对其进行聚类分析和相似度分析。结果建立了钩吻的指纹图谱测定方法,该方法精密度、重复性、稳定性良好。利用该方法对不同产地来源样品进行主成分和聚类分析,结果显示9批不同产地的钩吻药材成分大致可分为四类,不同产地来源的钩吻其内在化学成分均有差异,呈现出不同的分类。结论指纹图谱技术可为判断体外钩吻不同产地来源提供分类依据。Objective To establish HPLC fingerprint of gelsemium for its different source analysis. Methods 9 batches of gelsemium collected from Guangxi, Hubei, Zhejiang and Fujian provinces were studied on their similarities. HPLC method was employed with Welchrom C 18 column, and a mixture liquid of acetonitrile (A) and 0.025% trimethylamine (B) as mobile phase in a gradient elution (0 min, 0.5%A; 5 min, 1%A; 10 min, 3%A; 15 min, 8%A; 20 min, 15%A; 40 min, 30%A; 46 min, 36%A; 60 min, 65%A), at a flow rate of 1.0 mL/min, column temperature of 30℃ and detection wavelength of 272 nm. 1 g of gelsemium plant sample was boiled in 45 mL of water for 2 hours and was concentrated by vortex filtration through a 0.45 Bm microporous membrane. The HPLC fingerprints were analyzed in cluster. The sample precision, repeatability and stability were tested for at least 6 times. Results The HPLC fingerprint method was established with good precision, repeatability and stability, effective for the principal component analysis and cluster analysis of different-origin samples of gelsemium. 9 groups of gelsemium from different origin could be broadly divided into four categories. Gelsemium of varied sources differs in its intrinsic chemical composition, showing a different classification in SPSS. Conclusions The HPLC fingerprint technology could provide the basis for the source analysis of gelsemium plants in vitro. Further characteristic study of the indicators is required in order to establish a more comprehensive and accurate evaluation method when involvement in poisoning cases.
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