本文選題：超高效液相色譜 + 四極桿-飛行時(shí)間質(zhì)譜　； 參考：《色譜》2016年05期

【摘要】：建立了超高效液相色譜-四極桿-飛行時(shí)間串聯(lián)質(zhì)譜(UPLC-Q-TOF/MS)快速篩查血液中10種毒物的檢測(cè)方法。用乙酸乙酯提取血液樣品,濃縮至近干后,用甲醇溶解定容,過(guò)0.22μm濾膜后,直接測(cè)定。目標(biāo)物經(jīng)ACQUITY UPLC@BEH C18色譜柱(100 mm×2.1 mm,1.7μm)分離,以甲醇和0.1%(v/v)甲酸水溶液為流動(dòng)相,梯度洗脫,四極桿飛行時(shí)間串聯(lián)質(zhì)譜電噴霧正離子模式檢測(cè),外標(biāo)法定量。結(jié)果表明:目標(biāo)物在10.0~500.0μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)為0.990 8~0.995 8,檢出限和定量限分別為1.0~2.0μg/L和4.0~8.0μg/L。在20.0、50.0和200.0μg/L 3個(gè)添加水平下的平均回收率為56.7%~83.0%,相對(duì)標(biāo)準(zhǔn)偏差為3.6%~8.9%。利用Agilent Mass Hunter PCDL Manager軟件建立常見毒物的數(shù)據(jù)庫(kù),并應(yīng)用于加標(biāo)樣品的篩查分析。該方法能快速篩查出添加的10種常見毒物,檢出率達(dá)100%,且保留時(shí)間偏差均小于0.1 min,質(zhì)量偏差均小于1 mDa,同位素豐度匹配得分、同位素間距得分和MS匹配得分均大于90,MS/MS圖譜匹配得分均大于70。該方法可用于法庭與臨床毒物分析。
[Abstract]:An ultra high performance liquid chromatography quadrupole time of flight tandem mass spectrometry (UPLC-Q-TOF/MS) was established for the rapid screening of 10 toxic substances in the blood. The blood samples were extracted with ethyl acetate and concentrated to the near dry. After 0.22 mu m filter membrane was dissolved with methanol, the target was directly measured by ACQUITY UPLC@BEH C18 column (100 mm * 2.1 mm, 1.7 u m). ) separation, using methanol and 0.1% (v/v) formic acid solution as mobile phase, gradient elution, quadrupole flight time tandem mass spectrometry electrospray ionization mode detection and external standard method. The results show that the linear relationship of target objects in the range of 10.0~500.0 g/L is good, the correlation coefficient is 0.990 8~0.995 8, and the detection limit and quantitative limit are 1.0~2.0, g/L and 4.0~8, respectively. The average recovery rate of.0 mu g/L. at the 3 adding levels of 20.0,50.0 and 200 mu g/L is 56.7%~83.0%. The relative standard deviation is 3.6%~8.9%. using Agilent Mass Hunter PCDL Manager software to establish the database of common toxicants, and is applied to screening and analysis of the labeled samples. This method can quickly screen out 10 common poisons added, and the detection rate is 1. 00%, and the retention time deviation is less than 0.1 min, the quality deviation is less than 1 mDa, isotopic abundance matching scores, isotopic distance scores and MS matching scores are more than 90, MS/MS map matching scores are more than 70., the method can be used for forensic and clinical toxicology analysis.

【作者單位】： 重慶市公安局物證鑒定中心;
【基金】：重慶市公安局科技攻關(guān)計(jì)劃項(xiàng)目(G2013-04)~~
【分類號(hào)】：R446.11;O657.63

【參考文獻(xiàn)】

相關(guān)期刊論文 前4條

1 余璐;宋偉;呂亞寧;趙暮雨;周芳芳;胡艷云;鄭平;;超高效液相色譜-四極桿-飛行時(shí)間質(zhì)譜法快速篩查茶葉中的204種農(nóng)藥殘留[J];色譜;2015年06期

2 石銀濤;馮柏霖;王繪軍;郭t熺，

本文編號(hào)：1877507