超高效液相色谱-四极杆-飞行时间质谱法快速筛查血液中10种常见毒物

发布时间：2018-05-12 06:32

本文选题：超高效液相色谱 + 四极杆-飞行时间质谱　；参考：《色谱》2016年05期

【摘要】：建立了超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF/MS)快速筛查血液中10种毒物的检测方法。用乙酸乙酯提取血液样品,浓缩至近干后,用甲醇溶解定容,过0.22μm滤膜后,直接测定。目标物经ACQUITY UPLC@BEH C18色谱柱(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%(v/v)甲酸水溶液为流动相,梯度洗脱,四极杆飞行时间串联质谱电喷雾正离子模式检测,外标法定量。结果表明:目标物在10.0~500.0μg/L范围内线性关系良好,相关系数为0.990 8~0.995 8,检出限和定量限分别为1.0~2.0μg/L和4.0~8.0μg/L。在20.0、50.0和200.0μg/L 3个添加水平下的平均回收率为56.7%~83.0%,相对标准偏差为3.6%~8.9%。利用Agilent Mass Hunter PCDL Manager软件建立常见毒物的数据库,并应用于加标样品的筛查分析。该方法能快速筛查出添加的10种常见毒物,检出率达100%,且保留时间偏差均小于0.1 min,质量偏差均小于1 mDa,同位素丰度匹配得分、同位素间距得分和MS匹配得分均大于90,MS/MS图谱匹配得分均大于70。该方法可用于法庭与临床毒物分析。
[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.

【作者单位】：重庆市公安局物证鉴定中心;
【基金】：重庆市公安局科技攻关计划项目(G2013-04)~~
【分类号】：R446.11;O657.63

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