超高效液相色谱串联质谱法测定血清中百草枯及大鼠百草枯毒代动力学研究

[Determination of paraquat in serum by ultra performance liquid chromatography tandem mass spectrometry and toxicokinetics of paraquat in rat].

作者信息

Ma Jing, Li Hui, Zhang Jing, Yan Yongji, Ye Qiao, Shao Bing

机构信息

School of Public Health, Capital Medical University, Beijing 100069, China.

出版信息

Wei Sheng Yan Jiu. 2018 Nov;47(6):993-997.

PMID:30593335

Abstract

OBJECTIVE

To establish a simple and rapid ultra-performance liquid chromatography tandem mass spectrometry( UPLC-MS/MS) method for the determination of paraquat in serum, and to apply to the toxicokinetics of paraquat in rats.

METHODS

The samples separated on ACQUITY UPLC BEH HILIC column( 2. 1 mm × 50 mm, 1. 7 μm)with acetonitrile-50 mmol/L ammonium formate( 0. 4% formic acid) as mobile phase. The analytes were analyzed using ESI operating in the positive multiple reaction monitoring( MRM) mode. The method was used in toxicokinetic study in poisoned rat. Toxicokinetic parameters were calculated by WinNonlin 7. 0 statistical software.

RESULTS

Paraquat was linear in the range of 0. 3-1000. 0 μg/L, the recovery rate was 89. 0%-107. 7%, and the relative standard deviation( RSD) 1. 9%-13. 8%( n = 6). Toxicokinetic parameterswere as follows: C_(max), T_(max)and T_(1/2) were( 46. 50 ± 5. 11) mg/L, 0. 167 h, ( 63. 2 ±16. 2) h, respectively.

CONCLUSION

This method is highly sensitive, high accuracy and is suitable for the analysis of paraquat in the toxicokinetic study in rats.

摘要

目的

建立一种简单快速的超高效液相色谱串联质谱法（UPLC-MS/MS）测定血清中的百草枯，并将其应用于大鼠百草枯的毒代动力学研究。

方法

采用ACQUITY UPLC BEH HILIC柱（2.1 mm×50 mm，1.7μm），以乙腈-50 mmol/L甲酸铵（0.4%甲酸）为流动相进行样品分离。采用电喷雾离子源正离子模式下的多反应监测（MRM）对分析物进行检测。该方法用于中毒大鼠的毒代动力学研究。用WinNonlin 7.0统计软件计算毒代动力学参数。