本文關(guān)鍵詞： 干血斑 抗凝血?dú)⑹笏?液相色譜-串聯(lián)質(zhì)譜法 臨床中毒快檢　出處：《分析測試學(xué)報(bào)》2017年11期 　論文類型：期刊論文

【摘要】：為應(yīng)對臨床中毒快檢的需求,建立了干血斑樣本中12種抗凝血鼠藥的液相色譜-串聯(lián)質(zhì)譜定性定量方法。針對全打孔的干血斑樣本,考察了濾紙卡種類、潤濕步驟、提取溶劑種類對提取效果的影響。采用C18色譜柱進(jìn)行分離,以乙酸銨(5 mmol/L)水溶液-乙酸銨(5 mmol/L)甲醇溶液為流動(dòng)相進(jìn)行梯度洗脫,在電噴霧負(fù)離子電離方式下使用三重四極多反應(yīng)監(jiān)測模式檢測。結(jié)果表明,采用Whatman903濾紙卡為基底,以水為溶劑充分潤濕,再以含內(nèi)標(biāo)的甲醇溶液提取5 min,各鼠藥的提取率為66%~115%,且結(jié)果穩(wěn)定(日內(nèi)RSD小于15%)。除殺鼠酮的線性范圍為20~500 ng/m L(r2=0.998 7)外,其它11種鼠藥的線性范圍為5~500 ng/m L(r2=0.998 8~0.999 6);12種鼠藥的回收率為61%~105%,基質(zhì)效應(yīng)為71%~193%(日內(nèi)RSD小于15%)。該方法準(zhǔn)確、靈敏、快速且操作簡便,成功應(yīng)用于3例臨床鼠藥中毒病人樣本的快速檢測,為臨床毒物檢測和法醫(yī)毒物分析的快速篩查和準(zhǔn)確定量提供了新的技術(shù)方法。
[Abstract]:In order to meet the requirement of rapid detection of clinical poisoning, a qualitative and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS) for 12 kinds of anticoagulant rodents in dry blood spot samples was established. C18 chromatographic column was used for separation. The mobile phase was gradient elution with ammonium acetate 5 mmol / L aqueous solution and ammonium acetate 5 mmol / L methanol solution as mobile phase. The triple quadrupole multipole reaction monitoring mode was used in the electrospray anion ionization mode. The results showed that the Whatman903 filter card was used as the substrate and the water as the solvent to fully wetting. The extraction rate of each rodenticide was 660.115 and the results were stable (RSD < 150.The linear range of rodentione was 200.500 ng/m / L ~ (2 +) 0.998 / 7). The linear range of the other 11 kinds of rodenticide was 5 #number0# ng/m / L ~ (0.998) 8 ~ 0.999 ~ (6) C ~ (12). The recovery rate of 12 kinds of rodenticide was 61 ~ 10 ~ 5 and the matrix effect was 71 ~ 1 ~ 19 ~ 3 ~ (th) (RSD was less than 1595). The method was accurate, sensitive, rapid and easy to operate. It has been successfully applied to the rapid detection of 3 clinical rodent poisoning patients, which provides a new technical method for rapid screening and accurate quantitative analysis of clinical poison and forensic toxicology.
【作者單位】： 軍事醫(yī)學(xué)科學(xué)院毒物藥物研究所抗毒藥物與毒理學(xué)國家重點(diǎn)實(shí)驗(yàn)室;軍事醫(yī)學(xué)科學(xué)院附屬醫(yī)院中毒救治科;
【基金】：全軍醫(yī)學(xué)科技“十三五”重大項(xiàng)目(AWS15J007))
【分類號(hào)】：O657.63;R99
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本文編號(hào)：1525412