超高效液相色谱-三重四极杆/复合线性离子阱质谱法同时快速测定血浆和尿液中84种有毒植物成分

采用超高效液相色谱-三重四极杆/复合线性离子阱的质谱联用技术，建立了同时快速测定血浆和尿液中84种有毒植物成分的方法。血浆样品经乙腈沉淀去蛋白和除磷脂、尿液样品经甲醇稀释后直接进样，以含0.1%（体积分数，下同）甲酸和2 mmol/L甲酸铵的97%乙腈水溶液、含0.1%甲酸的2 mmol/L甲酸铵水溶液作为流动相进行梯度洗脱，在Acquity BEH C₁₈色谱柱上实现分离，在电喷雾正离子多离子监测触发的增强子离子扫描（MRM-IDA-EPI）模式下检测，基质工作曲线内标法定量。血浆和尿液中84种待测物在相应的浓度范围内线性关系良好，相关系数均大于或等于0.9911，血浆和尿液中的检出限（S/N=3）分别为0.01~1和0.03~2 μg/L，准确度（平均加标回收率）为70.6%~124.5%，日内和日间精密度分别为0.7%~18.4%和1.1%~18.5%。该法简单、快速、灵敏、准确，可用于血浆和尿液中84种有毒植物成分的中毒检测。

Simultaneous rapid determination of 84 toxic plant constituents in plasma and urine by ultra-performance liquid chromatography- triple quadrupole/linear ion trap mass spectrometry

An ultra-performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry (UPLC-Qtrap MS) method was developed for the determination of 84 toxic plant constiuents in plasma and urine. Plasma was precipitated by acetonitrile to remove proteins and then passed through a Prime HLB SPE column to remove phospholipids, while urine was diluted with methanol. Chromatographic separation of the analytes was achieved on an Acquity BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm) by gradient elution using the mobile phase of 0.1% (v/v) formic acid and 2 mmol/L ammonium formate both in 97% (v/v) acetonitrile aqueous solution and water. Electrospray ionization mass spectrometry was carried out in the positive ion mode with multiple reaction monitoring-information dependent acquisition-enhanced product ion scan mode (MRM-IDA-EPI). The 84 analytes were quantified by the matrix working standard curve internal standard method, and a good linear relationship was observed, with correlation coefficients of ≥ 0.9911. The limits of detection (LODs) in plasma and urine were 0.01-1 μg/L and 0.03-2 μg/L, respectively. The intra- and inter-day precisions of these analytes were 0.7%-18.4% and 1.1%-18.5%, and the accuracy of all analytes ranged from 70.6% to 124.5%. This method is simple, sensitive, and accurate for the measurement of these analytes in plasma and urine for both clinical and forensic applications.