涉案硝氯酚的色谱-质谱法快速检验

Rapid Detection of Niclofolan with Chromatography-mass Spectrometry

目的建立超高效液相色谱-串联四级杆飞行时间质谱(UPLC-QTOF)和气相色谱-质谱(GC-MS)技术联合鉴定检材中硝氯酚的方法。方法加标样品经甲醇提取,取上清液,采用UPLC-QTOF和GC-MS进行分析。结果GC-MS检测硝氯酚需要较高进样温度和较长时间得到特征碎片(344,326,298,268和160),且NIST 17中无该物质信息,易出现漏检。经UPLC-QTOF检测,保留时间4.99min,硝氯酚的[M-H]^-峰为m/z 342.9538,碰撞诱导解离(CID)模式下二级质谱主要离子有m/z 296.9611,295.9529,260.9835,214.9903,279.9576,249.9598。结论在目前缺少硝氯酚色谱-质谱检测信息且国内报道较少的情况下,本文为硝氯酚快速检测提供参考。

Objective To establish a method for identification of riclofolan by both GC-MS and PLC-QTOF The sample was extracted with methanol,centrifuged to have the supernatant being subjected to analysis with GC-MS and UPLC-QTOF.Results For the GC-MS choice,niclofolan was necessary of undergoing into injection at higher temperature and longer time processing so as to have it detected,appearing its characteristic fragment ion peaks at m/z 344,326,298,268 and160,yet no information obtained about it in the existing NIST 17,thus very prone to lead a missed check.In contrast,UPLCQTOF method was able to determine niclofolan,showing of the niclofolan being retention time of 4.99 min,its characteristic fragment ion peaks[M-H]^-(m/z 342.9538)in the single stage and m/z 296.9611,295.9529,260.9835,214.9903,279.9576,249.9598 in the tandem(MS/MS)mode.Conclusion For the present lack of relevant information about the detection of niclofolan to cause difficulty of getting assistance,this paper should be providing a reference for the rapid detection of niclofolan.