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血清和尿液中4種鵝膏肽類毒素的UPLC-ESI-Q-TOF分析

發(fā)布時(shí)間:2018-04-11 08:14

  本文選題:α-鵝膏毒肽 + β-鵝膏毒肽; 參考:《現(xiàn)代預(yù)防醫(yī)學(xué)》2017年23期


【摘要】:目的建立血清和尿液中α-鵝膏毒肽、β-鵝膏毒肽、二羥鬼筆毒肽、羧基二羥鬼筆毒肽毒素的超高效液相色譜-四級桿飛行時(shí)間串聯(lián)質(zhì)譜測定方法。方法血清樣品先用乙腈沉淀蛋白,再用含0.1%TFA的二氯甲烷提取,殘?jiān)煤?mmol/L乙酸銨的甲醇-水(30∶70)溶解;尿液樣品直接過0.22μm微孔濾膜;樣品溶液經(jīng)HSS T3色譜柱分離后用Q-TOF MS進(jìn)行測定。結(jié)果毒素準(zhǔn)分子離子準(zhǔn)確質(zhì)量數(shù)及其同位素特征、色譜峰保留時(shí)間可作為毒素定性鑒定的依據(jù),血清和尿液樣品的檢出限分別為10 ng/ml和5 ng/ml,定量限為20 ng/ml和10 ng/ml,加標(biāo)回收率分別為77.4%~95.6%和73.8%~103.8%,相對標(biāo)準(zhǔn)偏差在3.0%~18.0%和1.2%~25.4%之間。應(yīng)用該方法測定了大鼠染毒尿液中鵝膏肽類毒素。結(jié)論本方法簡便、準(zhǔn)確、可靠,適用于中毒事件生物樣品中4種鵝膏肽類毒素的檢測和確證分析。
[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.
【作者單位】: 深圳市南山區(qū)疾病預(yù)防控制中心;
【基金】:深圳市科技創(chuàng)新委科技研發(fā)資金基礎(chǔ)研究項(xiàng)目(JCYJ20140416095154396)
【分類號】:R155.3;R446.1

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