超高效液相色谱串联质谱法同时快速检验血液中3种哌嗪类新型毒品
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摘要
目的建立血液中3种哌嗪类新型毒品超高效液相色谱-三重四级杆质谱(UPLC-TQ/MS)快速检验方法。方法采用固相支撑液液萃取前处理方法,全血样品过柱后,用乙酸乙酯进行洗脱,氮吹浓缩后用初始流动相定容,Waters T3色谱柱分离,0.1%甲酸水和乙腈进行梯度洗脱。采用电喷雾电离,正离子(ESI+)模式扫描,多反应监测(MRM)模式检测。结果三种药物在1～500 ng/mL范围内呈良好线性关系(R~2≥0.999),回收率为92.3%～105.3%,相对标准偏差为0.7%～3.7%,方法检出限(S/N=3)为0.04～0.13 ng/mL,定量限(S/N=10)在0.13-0.43 ng/mL范围内。结论该方法能够满足实际办案快速、准确的需求。
Objective A fast testing method was established for the determination of BZP、TFMPP and mCPP in blood by ultra performance liquid chromatography tandem electrospray ionization triple quadrapole-mass spectrometry(UPLC-TQ/MS). Methods The LLE method was used for sample preparation. The blood samples were extracted with Ethyl acetate after p passing through a solid phase, the pretreated samples were concentrated by nitrogen and then the volume was determined by the initial mobile phase. Then the samples were separated through a Waters T3 column and were eluted with a gradient program with 0.1% formic acid-0.1% formic acid/acetonitrile as mobile phase, scanned with positive ions mode(ESI+), detected under multiple reaction monitoring(MRM) mode. Results As a result, zopiclone and its two metabolites displayed excellent linearity in the concentration of 1～500 ng/mL(R~2>0.999).The average recoveries ranged from 92.3% to 105.3%. The RSD were in the range of 0.7%～3.7%. Besides, the limit of detection(LOD) of this method for target drugs was 0.04～0.13 ng/mL(S/N=3), while the limits of quantification(LOQ)were in the range of 0.13-0.43 ng/mL(S/N=10). Conclusion This method can meet the demand of rapidity and accuracy in actual cases.
Objective A fast testing method was established for the determination of BZP、TFMPP and mCPP in blood by ultra performance liquid chromatography tandem electrospray ionization triple quadrapole-mass spectrometry(UPLC-TQ/MS). Methods The LLE method was used for sample preparation. The blood samples were extracted with Ethyl acetate after p passing through a solid phase, the pretreated samples were concentrated by nitrogen and then the volume was determined by the initial mobile phase. Then the samples were separated through a Waters T3 column and were eluted with a gradient program with 0.1% formic acid-0.1% formic acid/acetonitrile as mobile phase, scanned with positive ions mode(ESI+), detected under multiple reaction monitoring(MRM) mode. Results As a result, zopiclone and its two metabolites displayed excellent linearity in the concentration of 1～500 ng/mL(R~2>0.999).The average recoveries ranged from 92.3% to 105.3%. The RSD were in the range of 0.7%～3.7%. Besides, the limit of detection(LOD) of this method for target drugs was 0.04～0.13 ng/mL(S/N=3), while the limits of quantification(LOQ)were in the range of 0.13-0.43 ng/mL(S/N=10). Conclusion This method can meet the demand of rapidity and accuracy in actual cases.
引文
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[2]Nikolova I,Danchev N.Piperazine-based substances of abuse:A new party pills on bulgarian drug market[J].Biotechnology&Biotechnological Equipment,2008,22:652-655.
[3]Baumann MH,Clark RD,Budzynski AG,et al.N-Substituted piperazines abused by humans mimic the molecular mechanism of 3,4-Methylene dioxymethamphetamine(MDMA,or“Ecstasy”)[J].Neuro psychopharmacology,2005,30550-560.
[4]徐多麒,张蕾萍,王继芬,等.超高效液相色谱串联质谱法同时快速检验全血中扎来普隆及其代谢产物[J].分析化学,2016,44(7):1059-1064.