气相色谱-质谱法快速检测全血和尿液中百草枯、敌草快

何宗剑; 朱定姬; 朱杰; 黄克建

doi:10.16369/j.oher.issn.1007-1326.2020.04.025

气相色谱-质谱法快速检测全血和尿液中百草枯、敌草快

Rapid detection of paraquat and diquat in whole blood and urine by gas chromatography-mass spectrometry

摘要

摘要:
目的建立测定全血、尿液中百草枯和敌草快的气相色谱-质谱（GC-MS）方法。
方法以乙基百草枯为内标，含体积分数10%高氯酸的乙醇溶液沉淀蛋白，加入硼氢化钠-氯化镍还原体系，在60℃下还原反应40 min，经1.0 mL乙酸乙酯萃取，在GC-MS选择离子监测模式（SIM）下测定。
结果百草枯、敌草快在质量浓度范围0.05~2.0 μg/mL（全血）、0.02~2.0 μg/mL（尿液）内的线性关系良好，相关系数分别为0.999 5~0.999 9，方法检出限分别为0.004~0.008 μg/mL，加标回收率为94.1%~115.0%，相对标准偏差（RSD）为1.1%~6.6%。全血、尿液中百草枯和敌草快在4℃冰箱中至少可以保存7 d。
结论该方法简单准确、灵敏度高，能够满足全血和尿液样品中百草枯、敌草快的快速检测。

Abstract:
Objective To establish a method for determination of paraquat and diquat in whole blood and urine by gas chromatography-mass spectrometry(GC-MS).
Methods Ethyl paraquat was used as internal standard, 10% perchloric acid-ethanol solution (V/V) was added to precipitate protein, and sodium borohydride-nickel chloride(NaBH₄-NiCl₂) were used in the reduction system. The reaction time was 40 minutes at 60℃, then the analytes were extracted with 1.0 mL ethyl acetate, and finally detected in GC-MS selective ion monitoring mode(SIM).
Results The linearities were good within investigated mass concentration ranges of 0.05 to 2.0 μg/mL in the whole blood and 0.02 to 2.0 μg/mL in urine of the paraquat and diquat. The correlation coefficients were 0.999 5 to 0.999 9, the detection limits of the method were 0.004 to 0.008 μg/mL, and the recoveries at three spiked levels were within 94.1%-115.0%, with 1.1%-6.6% of the relative standard deviation (RSD). Paraquat and diquat in blood and urine could be stored for at least 7 days at 4℃.
Conclusion The established method is simple, accurate, and sensitive for rapid detection of paraquat and diquat in whole blood and urine samples.

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