【摘要】：目的建立同時檢測血液中氨曲南及甲硝唑的超高效液相色譜串聯(lián)質(zhì)譜分析方法。方法以頭孢拉定和氯霉素為內(nèi)標(biāo),血液樣品經(jīng)乙腈沉淀蛋白后通過高效液相色譜分離,電噴霧離子源進(jìn)行離子化,采用多反應(yīng)監(jiān)測方式(multiple reaction monitoring mode,MRM)對各化合物進(jìn)行監(jiān)測。結(jié)果所建立的方法可同時檢測血液中的氨曲南和甲硝唑成分,氨曲南在10~5 000 ng/mL、甲硝唑在1~1 000 ng/mL的線性范圍內(nèi)具有良好的線性關(guān)系,線性相關(guān)系數(shù)r均大于0.995;血液中氨曲南和甲硝唑的檢出限分別為5和0.5 ng/mL(S/N=3∶1);定量限分別為10和1 ng/mL(S/N=10∶1);方法的日間及日內(nèi)精密度均小于10%,準(zhǔn)確度為89.6%~97.5%。將此方法應(yīng)用于1例醫(yī)療糾紛案件的鑒定,在涉案死者的血液中同時檢出氨曲南及甲硝唑成分,血液中氨曲南及甲硝唑的質(zhì)量濃度分別為438 ng/mL和15μg/mL。結(jié)論本研究所建立的分析方法靈敏度高、簡便快速、專屬性強(qiáng)、可靠性高,為司法鑒定實踐中涉及氨曲南和甲硝唑的案件提供了技術(shù)支持和基礎(chǔ)數(shù)據(jù)。
[Abstract]:OBJECTIVE To establish a method for simultaneous determination of aztreonam and metronidazole in blood by ultra-high performance liquid chromatography tandem mass spectrometry.METHODS Cefradine and chloramphenicol were used as internal standard,protein was precipitated by acetonitrile and separated by high performance liquid chromatography,ionized by electrospray ionization,and multi-reaction monitoring was used. Results The established method could simultaneously detect aztreonam and metronidazole in blood. The linear relationship between aztreonam and metronidazole was good in the linear range of 10-5 000 ng/mL, 1-1 000 ng/mL, and the linear correlation coefficient r was greater than 0.995. The quantitative limits were 10 ng/mL and 1 ng/mL (S/N=10:1), respectively, and the intra-day and intra-day precision were less than 10% and 89.6% ~ 97.5% respectively. CONCLUSION The method is sensitive, simple, rapid, specific and reliable. It provides technical support and basic data for the cases involving aztreonam and metronidazole in forensic practice.
【作者單位】： 司法部司法鑒定科學(xué)技術(shù)研究所上海市法醫(yī)學(xué)重點實驗室上海市司法鑒定專業(yè)技術(shù)服務(wù)平臺;
【基金】：十三五國家重點研發(fā)計劃項目(2016YFC0800700-4) 國家自然科學(xué)基金青年項目(81501633) 上海市法醫(yī)學(xué)重點實驗室項目(17DZ2273200) 上海市司法鑒定專業(yè)技術(shù)服務(wù)平臺資助項目(16DZ2290900)~~
【分類號】：D919
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本文編號：2232291