色谱

色谱 ›› 2016, Vol. 34 ›› Issue (5): 538-542.DOI: 10.3724/SP.J.1123.2016.01028

• 技术与应用 • 上一篇    

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

石银涛, 王绘军, 郭璟琦, 丁静, 王俊伟   

  1. 重庆市公安局物证鉴定中心, 重庆 400021
  • 收稿日期:2016-01-22 出版日期:2016-05-08 发布日期:2012-12-18
  • 通讯作者: 王俊伟
  • 基金资助:

    重庆市公安局科技攻关计划项目(G2013-04).

Rapid screening of 10 drugs in blood using ultra performance liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry

SHI Yintao, WANG Huijun, GUO Jingqi, DING Jing, WANG Junwei   

  1. Institute of Forensic Science, Public Security Department of Chongqing, Chongqing 400021, China
  • Received:2016-01-22 Online:2016-05-08 Published:2012-12-18
  • Supported by:

    Key Science and Technology Program of Chongqing City Public Security Bureau (No. G2013-04).

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被引次数

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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0.22 μ m滤膜后,直接测定。目标物经ACQUITY UPLC@BEH C18 色谱柱(100 mm×2.1 mm, 1.7 μ m)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10.0~500.0 μ g/L范围内线性关系良好,相关系数为0.9908~0.9958,检出限和定量限分别为1.0~2.0 μ g/L和4.0~8.0 μ g/L。在20.0、50.0和200.0 μ g/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。

关键词: 超高效液相色谱, 毒物, 快速筛查, 四极杆-飞行时间质谱, 血液

Abstract:

A high-throughput method was developed for rapid screening of 10 drugs in blood by ultra performance liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS). The sample was extracted by ethyl acetate, the extraction solution was concentrated to near dryness, and dissolved with methanol. Then the sample was passed through a 0.22 μ m membrane. The separation of the 10 target compounds was performed on a Waters ACQUITY UPLC@BEH C18 column (100 mm×2.1 mm, 1.7 μ m) with gradient elution using methanol and 0.1% (v/v) formic acid aqueous solution as mobile phases, and analyzed by UPLC-Q-TOF/MS under electrospray ionization (ESI) mode with scanning range of m/z 50-1000. Rapid screening can be achieved using MS matching scores, deviation of retention time, measured mass, isotopic abundance matching scores, isotope spacing match scores and MS/MS matching scores. Good linearities were observed in the range of 10.0-500.0 μ g/L with the correlation coefficients from 0.9908 to 0.9958. The limits of detection and the limits of quantification were 1.0-2.0 μ g/L and 4.0-8.0 μ g/L, respectively. The spiked recoveries were 56.7%-83.0% with the relative standard deviations of 3.6%-8.9%. The result screening database was built using Agilent Mass Hunter PCDL Manager software and then used for the analysis of spiked samples. MS matching scores, isotopic abundance matching scores, isotope spacing matching scores (all > 90 points) and MS/MS matching scores (> 70 points) were applied to identify the drugs. The results showed that all the spiked drugs could be correctly identified with low deviations of retention time (< 0.1 min) and mass (< 1 mDa). The developed method is suitable for the screening and confirmation of the drugs in forensic and clinical analytical toxicology.

Key words: blood, drugs, quadrupole-time-of-flight mass spectrometry (Q-TOF/MS), rapid screening, ultra performance liquid chromatography (UPLC)

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