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开发并验证了一种灵敏、高通量的 UPLC-MS/MS 方法,用于测定人血浆和尿液中的百草枯和敌草快:应用于医院急诊科中毒病例。

Development and validation of a sensitive and high throughput UPLC-MS/MS method for determination of paraquat and diquat in human plasma and urine: application to poisoning cases at emergency departments of hospitals.

机构信息

Department of Forensic Medicine, Nanjing Medical University, Nanjing, Jiangsu, 211166, People's Republic of China.

Jiangsu Province Hospital, The First Affiliated Hospital of Nanjing Medical University, Nanjing, China.

出版信息

Forensic Toxicol. 2022 Jan;40(1):102-110. doi: 10.1007/s11419-021-00603-9. Epub 2021 Nov 12.

Abstract

PURPOSE

Paraquat and diquat are well-known toxic herbicides, at least responsible for hundreds of fatal poisoning events worldwide. However, the determination of diquat and paraquat in plasma and urine is very challenging because of their high polarity and double charge characteristics. In this study, we aim to develop a rapid and reliable method for the determination of paraquat and diquat in human plasma and urine by ultraperformance liquid chromatography-tandem mass spectrometry.

METHOD

The chromatographic separation of paraquat and diquat was tested with different chromatographic columns and different mobile phase conditions. The mass parameters were optimized by product ions, source gas flow, cone flow, desolvation temperature, and capillary voltage. The isocratic elution mode gave rapid appearance of peak of paraquat and diquat.

RESULTS

The sharp peak shapes for paraquat and diquat were achieved with CORTECS UPLC HILIC (100 × 2.1 mm, 1.6 μm) column by adding formic acid and ammonium acetate in mobile phase in isocratic elution mode. The lower limit of quantification of 1.0 ng/mL for paraquat and diquat were achieved using only 50 μL of human plasma or urine. The running time for analysis of both paraquat and diquat was as short as 3.5 min per sample.

CONCLUSIONS

A rapid and reliable method for the determination of paraquat and diquat was developed and applied to 387 clinical poisoning cases and 22 poisoning cases were found to be paraquat or diquat poisoning.

摘要

目的

百草枯和敌草快是众所周知的有毒除草剂,至少在全球范围内造成了数百起致命中毒事件。然而,由于其高极性和双电荷特性,在血浆和尿液中测定百草枯和敌草快非常具有挑战性。本研究旨在开发一种快速可靠的超高效液相色谱-串联质谱法测定人血浆和尿液中百草枯和敌草快的方法。

方法

用不同的色谱柱和不同的流动相条件测试了百草枯和敌草快的色谱分离。通过产物离子、气源流量、锥流、脱溶温度和毛细管电压优化了质谱参数。等度洗脱模式使百草枯和敌草快的峰迅速出现。

结果

在等度洗脱模式下,通过在流动相中添加甲酸和乙酸铵,在 CORTECS UPLC HILIC(100×2.1mm,1.6μm)柱上实现了百草枯和敌草快的尖锐峰形。百草枯和敌草快的定量下限均为 1.0ng/mL,仅需 50μL 人血浆或尿液即可达到。分析百草枯和敌草快的运行时间均为每个样品 3.5 分钟。

结论

建立了一种快速可靠的测定百草枯和敌草快的方法,并应用于 387 例临床中毒病例,发现 22 例为百草枯或敌草快中毒。

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