超高效液相色谱-串联四极杆飞行时间质谱法筛查人全血中150种药物与毒物
Screen-Testing of 150 Drugs and Toxic Compounds in Human Whole Blood by UPLC-TOF/MSE
摘 要
采用超高效液相色谱-串联四极杆飞行时间质谱法(UPLC-TOF/MSE)筛查人全血中的150种药物与毒物。人全血样品经液液萃取后,用ACQUITY UPLC HSS C18色谱柱分离,以不同体积比的pH 3.0的5 mmol·L-1甲酸铵溶液以及1%(体积分数)甲酸-乙腈溶液的混合液为流动相进行梯度洗脱,质谱采用电喷雾电离正离子模式全扫描筛查。150种药物与毒物的检出限(3S/N)在0.2~25 μg·L-1之间。67种化合物的基质效应在17.4%~126%之间,提取回收率在29.7%~114%之间。
人全血
药物
毒物
UPLC-TOF/MSE
Human whole blood
Drugs
Toxic compounds
Abstract
UPLC-TOF/MSE was applied to the screen-testing of 150 drugs and toxic compounds in human whole blood. The human whole blood sample was prepared by liquid-liquid extraction, then separated on ACQUITY UPLC HSS C18 column. Mixtures of 5 mmol·L-1 ammonium formate solution (pH 3.0) and 1% (φ) formic acid-acetonitrile solution mixed in different ratios were used as mobile phase in gradient elution. Modes of positive electric spray ionization and full-scanning were adopted in MS. Detection limits (3S/N) of the 150 drugs and toxic compounds found were in the range of 0.2-25 μg·L-1. Matrix effects for 67 compounds were found in the range of 17.4% to 126%, and values of recovery of liquid-liquid extraction were ranged from 29.7% to 114%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201604010
所属栏目 工作简报
基金项目
收稿日期 2015/9/28
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备注姜凤丽(1989-),女,山东菏泽人,硕士研究生,研究 方向为体内毒物分析。
引用该论文: JIANG Feng-li,TENG Xiao-mei,NI Chun-fang,LIANG Chen,WANG Rong,ZENG Li-bo,ZHANG Yu-rong. Screen-Testing of 150 Drugs and Toxic Compounds in Human Whole Blood by UPLC-TOF/MSE[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(4): 417～426
姜凤丽,滕小梅,倪春芳,梁 晨,汪 蓉,曾立波,张玉荣. 超高效液相色谱-串联四极杆飞行时间质谱法筛查人全血中150种药物与毒物[J]. 理化检验－化学分册, 2016, 52(4): 417～426
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参考文献
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【2】KERRIGAN S, MELLON M B, BANUELOS S, et al. Evaluation of commercial enzyme-linked immunosorbent assays to identify psychedelic phenethylamines［J］. J Anal Toxicol, 2011,35(7):444-451.
【3】RAMOO B, FUNKE M, FRAZEE C, et al. Comprehensive urine drug screen by gas chromatography/mass spectrometry (GC/MS)［J］. Methods Mol Biol, 2016,1383:125-131.
【4】MADEJ K, PERSONA K, WANDAS M, et al. Sequential cloud-point extraction for toxicological screening analysis of medicaments in human plasma by high pressure liquid chromatography with diode array detector［J］. J Chromatogr A, 2013,1312:42-48.
【5】PEDERSEN A J, DALSGAARD P W, RODE A J, et al. Screening for illicit and medicinal drugs in whole blood using fully automated SPE and ultra-high-performance liquid chromatography with TOF-MS with data-independent acquisition［J］. J Sep Sci, 2013,36(13):2081-2089.
【6】王飞,陈其勇,宓捷波,等.超高效液相色谱-串联质谱法测定畜产品中6种青霉素类药物残留［J］.理化检验-化学分册, 2015,51(6):756-760.
【7】VIETTE V, FATHI M, RUDAZ S, et al. Current role of liquid chromatography coupled to mass spectrometry in clinical toxicology screening methods［J］. Clin Chem Lab Med, 2011,49(7):1091-1103.
【8】STURM S, HAMMANN F, DREWE J, et al. An automated screening method for drugs and toxic compounds in human serum and urine using liquid chromatography-tandem mass spectrometry［J］. J Chromatogr B, 2010,878(28):2726-2732.
【9】BJRK M K, NIELSEN M K, MARKUSSEN L , et al. Determination of 19 drugs of abuse and metabolites in whole blood by high-performance liquid chromatography-tandem mass spectrometry［J］. Anal Bioanal Chem, 2010,396(7):2393-2401.
【10】ROSANO T G, WOOD M, IHENETU K, et al. Drug screening in medical examiner casework by high-resolution mass spectrometry (UPLC-MSE-TOF)［J］. J Anal Toxicol, 2013,37(8):580-593.
【11】LEE H K, HO C S, IU Y P, et al. Development of a broad toxicological screening technique for urine using ultra-performance liquid chromatography and time-of-flight mass spectrometry［J］. Anal Chim Acta, 2009,649:80-90.
【12】TENG X M, LIANG C, WANG R, et al. Screening of drugs of abuse and toxic compounds in human whole blood using online solid-phase extraction and high-performance liquid chromatography with time-of-flight mass spectrometry［J］. J Sep Sci, 2015,38(1):51-59.
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