Zhou Yan, He Ming-Fang, Choi Franky Fung-Kei, He Zhi-Heng, Song Jing-Zheng, Qiao Chun-Feng, Li Song-Lin, Xu Hong-Xi
Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu, China.
Biomed Chromatogr. 2011 Aug;25(8):851-7. doi: 10.1002/bmc.1534. Epub 2010 Nov 5.
A high-sensitivity ultra-performance liquid-chromatography (UPLC) coupled with tandem mass spectrometric method was developed for simultaneous quantification and confirmation of triptolide in both zebrafish embryos and the aqueous-exposure solution on a tandem quadrupole mass spectrometer (TQ-MS). This was achieved by performing quantification using the multiple reaction monitoring (MRM) acquisition with simultaneous characterization of the MRM peak using product ion confirmation (PIC) acquisition as it elutes from the chromatographic system. Separation was achieved on a 1.7 µm C(18) UPLC column using 0.1% formic acid water-acetonitrile mobile phase with a cycle time of 6 min. The linear range of 0.115-360 ng/mL, and lower limits of detection of 0.02 ng/mL and quantification of 0.064 ng/mL were established. This method was successfully applied to determine the time course of triptolide absorption by zebrafish embryos and the amount of triptolide remaining in the culture medium after administration of two triptolide dosages at three time points. This coupled MRM with PIC approach could provide both qualitative and quantitative results without the need for repetitive analyses. This resulted in the reduction of further confirmative experiments and analytical time, and ultimately increased laboratory productivity.
建立了一种高灵敏度超高效液相色谱（UPLC）与串联质谱联用的方法，用于在串联四极杆质谱仪（TQ-MS）上同时定量和确证斑马鱼胚胎及水暴露溶液中的雷公藤甲素。这是通过使用多反应监测（MRM）采集进行定量，并在其从色谱系统洗脱时使用产物离子确证（PIC）采集对MRM峰进行同时表征来实现的。在1.7 µm C(18) UPLC柱上，使用0.1%甲酸水-乙腈流动相，循环时间为6分钟实现分离。建立了0.115 - 360 ng/mL的线性范围，检测下限为0.02 ng/mL，定量下限为0.064 ng/mL。该方法成功应用于确定斑马鱼胚胎吸收雷公藤甲素的时间进程以及在三个时间点给予两种雷公藤甲素剂量后培养基中剩余的雷公藤甲素量。这种将MRM与PIC相结合的方法无需重复分析即可提供定性和定量结果。这减少了进一步的确证实验和分析时间，最终提高了实验室效率。
