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

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0.05~2.0μg/mL(全血)、0.02~2.0μg/mL(尿液)内的线性关系良好,相关系数分别为0.9995~0.9999,方法检出限分别为0.004~0.008μg/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。

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 acidethanol 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 2.0μg/mL in the whole blood and 0.02 to 2.0μg/mL in urine of the paraquat and diquat.The correlation coefficients were 0.9995 to 0.9999,the detection limits of the method were 0.004 to 0.008μg/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.