血清和尿液中4种鹅膏肽类毒素的UPLC-ESI-Q-TOF分析

发布时间：2018-04-11 08:14

本文选题：α-鹅膏毒肽 + β-鹅膏毒肽　；参考：《现代预防医学》2017年23期

【摘要】：目的建立血清和尿液中α-鹅膏毒肽、β-鹅膏毒肽、二羟鬼笔毒肽、羧基二羟鬼笔毒肽毒素的超高效液相色谱-四级杆飞行时间串联质谱测定方法。方法血清样品先用乙腈沉淀蛋白,再用含0.1%TFA的二氯甲烷提取,残渣用含2mmol/L乙酸铵的甲醇-水(30∶70)溶解;尿液样品直接过0.22μm微孔滤膜;样品溶液经HSS T3色谱柱分离后用Q-TOF MS进行测定。结果毒素准分子离子准确质量数及其同位素特征、色谱峰保留时间可作为毒素定性鉴定的依据,血清和尿液样品的检出限分别为10 ng/ml和5 ng/ml,定量限为20 ng/ml和10 ng/ml,加标回收率分别为77.4%~95.6%和73.8%~103.8%,相对标准偏差在3.0%~18.0%和1.2%~25.4%之间。应用该方法测定了大鼠染毒尿液中鹅膏肽类毒素。结论本方法简便、准确、可靠,适用于中毒事件生物样品中4种鹅膏肽类毒素的检测和确证分析。
[Abstract]:Methods Serum samples were precipitated with acetonitrile and then extracted with dichloromethane containing 0.1%TFA. The residue was dissolved with methanol-water 30: 70 containing ammonium 2mmol/L acetate.The sample solution was separated by HSS T3 column and determined by Q-TOF MS.Results the accurate mass number and isotopic characteristics of toxin excimer ions and the retention time of chromatographic peak can be used as the basis for the qualitative identification of toxins.The method was used to determine the peptide toxins in the urine of rats exposed to ointment.Conclusion this method is simple, accurate and reliable. It is suitable for the detection and identification of four kinds of peptide toxins in the biological samples of poisoning events.
【作者单位】：深圳市南山区疾病预防控制中心;
【基金】：深圳市科技创新委科技研发资金基础研究项目(JCYJ20140416095154396)
【分类号】：R155.3;R446.1

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