Objective To establish a rapid analytical method for determination of 1-(4-methoxyphenyl)piperazine (MeOPP) in whole blood based on liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry (LC-QTrap-MS/MS). Methods The blood samples were treated with acetonitrile under oscillation, afterwards centrifugalized to precipitate the offal, with the supernatant being received as the analyte that was subjected to LC-QTrap-MS/MS analysis. LC was conducted within 5.5min via a Phenomenex Kinetx®5.0μm Biphenyl 100Å (100mm×2.1mm) column that was kept at 40℃ of oven temperature and flowed at 0.5mL/min with a gradient elution of the mobile phase consisting of 0.1% formic acid aqueous solution - acetonitrile. The multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) scanning was adopted for determination of the analyte. 1-(4-methoxyphenyl)piperazine harbored in whole blood was quantitatively detected against its calibration curve. Results 1-(4-methoxyphenyl)piperazine, spiked in human blood samples, showed good linearity from its calibration curve over the concentration range from 2~200ng/mL under the optimized MS-MS conditions, having a maximal correlation coefficient of 0.9984 and the extraction recoveries achieved up to 87%, plus the intra- and inter-day relative standard deviations (RSDs) lower than 5% and 10%, respectively. In addition, its limit of detection (LOD) and limit of quantification (LOQ) were individually 0.8ng/mL and 2ng/mL. Conclusions LC-QTrap-MS/MS, assisted with MRM-IDA-EPI mode, can retain the same sensitivity as MRM's for quantification, yet having more abundant information provided about secondary fragment ions so as to make the qualitative Results more accurate. The here-developed method is simple, fast, accurate, specific, high of recovery rate and good of reproducibility, suitable for simultaneous qualitative and quantitative analysis of 1-(4- methoxyphenyl) piperazine in blood samples.
Key words
forensic toxicology /
liquid chromatography-triple quadrupole/linear ion trap tandem mass spectrometry (LC-QTrap-MS/MS) /
1-(4-methoxyphenyl)piperazine (MeOPP)
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