液相色谱-质谱法同时检测全血和尿液中草甘膦、草铵膦、敌草快和百草枯

何宗剑; 周萍; 卿郅聪; 朱定姬; 覃利梅; 宁攀良

doi:10.16369/j.oher.issn.1007-1326.2025.240341

液相色谱-质谱法同时检测全血和尿液中草甘膦、草铵膦、敌草快和百草枯

Simultaneous determination of glyphosate, glufosinate, diquat, and paraquat in whole blood and urine by liquid chromatography mass spectrometry

摘要

摘要:
目的建立同时检测全血和尿液中草甘膦（glyphosate，GLY）、草铵膦（glufosinate，GLUF）、敌草快（diquat，DQ）和百草枯（paraquat，PQ）的液相色谱-质谱法。
方法取0.5 mL全血加入0.2 mL超纯水、1.5 mL乙腈，取0.5 mL尿样加入0.5 mL超纯水，涡旋、超声萃取，以含20 mmol/L乙酸铵（pH值=3.0）水溶液和乙腈作为流动相，经Acclaim Trinity Q1色谱柱（3 mm×100 mm×3 μm）分离，质谱检测。
结果 4种除草剂在相应的质量浓度范围内线性关系良好，检出限范围0.001~0.087 mg/L。3个浓度水平的加标回收率为82.4%~115.5%，相对标准偏差为1.3%~9.9%。
结论建立的全血和尿液中4种除草剂测定方法操作简单、快速、灵敏度高，适用于中毒患者全血和尿液中GLY、GLUF、DQ、PQ的同时测定。

Abstract:
Objective To establish a liquid chromatography-mass spectrometry method for the simultaneous detection of glyphosate (GLY), glufosinate (GLUF), diquat (DQ), and paraquat (PQ) in whole blood and urine.
Methods 0.5 mL of whole blood was added to 0.2 mL of ultrapure water and 1.5 mL of acetonitrile, and 0.5 mL of urine was added to 0.5 mL of ultrapure water. Then the ultrasonically extracted was done after vortex shaking. An Acclaim Trinity Q1 column (3 mm×100 mm×3 μm) with a mobile phase of 20 mmol/L ammonium acetate (pH = 3.0) aqueous solution and acetonitrile was used for separation, followed by mass spectrometry detection.
Results The four herbicides showed good linear relationships within their respective concentration ranges, with detection limits ranging from 0.001 to 0.087 mg/L. The spiked recovery rates at three concentration levels ranged from 82.4% to 115.5%, with relative standard deviations of 1.3% to 9.9%.
Conclusions The established method for the determination of the four herbicides in whole blood and urine is simple, rapid, and highly sensitive, making it suitable for the simultaneous detection of GLY, GLUF, DQ, and PQ in the blood and urine of poisoned patients.

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