超高效液相色谱-串联四级杆飞行时间质谱法快速筛查尿液中58种毒品及滥用药物
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摘要
目的建立超高效液相色谱-串联四级杆飞行时间质谱(UPLC-Q-TOF/MSE)快速筛查人体尿液中58种毒品及滥用药物的方法。方法样品经甲醇蛋白沉淀法进行前处理。目标物经ACQUITY UPLC HSS C18色谱柱分离,以0.1%甲酸-乙腈溶液及5mmol/L甲酸铵-水溶液(pH=3)为流动相进行梯度洗脱,质谱采用电喷雾电离正离子全扫描模式(MSE)检测。利用UNIFI软件建立数据库,并对样品进行筛查分析。结果人体尿液中58种毒品及滥用药物的检出限(LOD,3S/N)在0.2～25.0ng/mL之间,用UNIFI软件对尿液样品中添加的58种毒品及滥用药物进行快速筛查,通过数据库比对,目标化合物均被检出。结论方法的准确性高,操作简单、快速,适用于尿液中毒品及滥用药物的快速筛查。
Objective To establish a method for rapid screening of 58 drugs in human urine by ultra-high performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF/MSE). Methods The spiked samples were pretreated by protein precipitation with methanol, thereby having the target compounds separated from Acquity UPLC HSS C18 column that was flowed through gradient elution of 0.1% formic acid-acetonitrile and 5 mmol/L ammonium formate-water(pH=3) mixture, the mobile phase. The electrospray ionization in positive ion was used for analysis in full scanning mode(MSE). UNIFI software was selected to set up the database and to process samples. Results The limit of detection(LOD, 3 S/N) for 58 drugs in human urine was in the range of 0.2～25.0 ng/ml. The target compounds were all detected by the established database from UNIFI software. Conclusions The method is accurate, simple and rapid, suitable for rapid screening of abused drugs in urine.
Objective To establish a method for rapid screening of 58 drugs in human urine by ultra-high performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF/MSE). Methods The spiked samples were pretreated by protein precipitation with methanol, thereby having the target compounds separated from Acquity UPLC HSS C18 column that was flowed through gradient elution of 0.1% formic acid-acetonitrile and 5 mmol/L ammonium formate-water(pH=3) mixture, the mobile phase. The electrospray ionization in positive ion was used for analysis in full scanning mode(MSE). UNIFI software was selected to set up the database and to process samples. Results The limit of detection(LOD, 3 S/N) for 58 drugs in human urine was in the range of 0.2～25.0 ng/ml. The target compounds were all detected by the established database from UNIFI software. Conclusions The method is accurate, simple and rapid, suitable for rapid screening of abused drugs in urine.
引文
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[12]姜凤丽,滕小梅,倪春芳,等.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.
[13]石银涛,王绘军,郭璟琦,等.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[J].色谱,2016,34(5):538-542.
[14]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].Journal of Separation Science Jss,2013,36(13):2081-2089.
[15]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.
[16]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].Journal of Chromatography A,2013,1312:42-48.
[2]雷红英.毒品犯罪现状、原因分析及对策建议--L县检察院办理毒品犯罪案件实证分析[J].法制博览,2018(32):148-149.
[3]王丹.中空纤维液相微萃取在检测阿片类毒品中的应用研究[D].北京:中国人民公安大学,2017.
[4]努尔艾力·塔依尔,毛新民,车文森,等.GC、GC-MS法定性定量法检测血液和尿液中阿片类毒品及其代谢物的含量[J],新疆医科大学学报,2016,39(7):849-857.
[5]杨崇俊,李强,高中勇,等.HS-SPME-GC/MS法检测尿液及毛发中苯丙胺类毒品[J],中国法医学杂志,2014,29(2):93-96.
[6]RAMOO B,FUNKE M,FRAZEE C,et al.Comprehensive urine drug screen by gas chromatography/mass spectrometry(GC/MS)[J].Clinical Applications of Mass Spectrometry in Drug Analysis,2016,1383:125-131.
[7]刘心,付饶,李敏,等.离子液体分散液相微萃取-毛细管电泳法检测尿液中的毒品[J],分析化学,2013,41(12):1919-1922.
[8]王燕燕,孟品佳,孟梁.毛细管电泳pH酸修饰在线富集方法检测唾液中鸦片类毒品[J],分析化学学报,2013,29(4):497-500.
[9]KERRIGAN S,MELLON M B,BANUELOS S,et al.Evaluation of commercial enzyme-linked immunosorbent assays to identify psychedelic phenethylamines[J].J Journal of Analytical Toxicology,2011,35(7):444-451.
[10]代勇,皮建华,周晓英.HPLC检测液相小体积提取唾液中的卡西酮类毒品[J],华西医学医学杂志,2015,30(5):598-600.
[11]BIRKLER R I,TELVING R,INGEMANN-HANSEN O,et al.Screening analysis for medicinal drugs and drugs of abuse in whole blood usingultra-performance liquid chromatography time-of-flight mass spectrometry(UPLC-TOF-MS)-toxicological findings in cases of alleged sexual assault[J].Forensic Science International,2012,222(1/3):154-161.
[12]姜凤丽,滕小梅,倪春芳,等.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.
[13]石银涛,王绘军,郭璟琦,等.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[J].色谱,2016,34(5):538-542.
[14]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].Journal of Separation Science Jss,2013,36(13):2081-2089.
[15]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.
[16]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].Journal of Chromatography A,2013,1312:42-48.