亲水超高效液相色谱-串联质谱法同时测定尿液中百草枯和敌草快

Simultaneous determination of Paraquat and Diquat in urine by hydrophilic ultra high performance liquid chromatography-tandem mass spectrometry

建立亲水超高效液相色谱-串联质谱法同时测定尿液中百草枯和敌草快的方法。样品经磷酸盐缓冲液(pH=6.8)提取,用弱阳离子交换固相萃取柱净化,选择Waters HILIC色谱柱(100 mm×2.1 mm,1.7μm)为分离柱,以乙腈-200 mmol/L甲酸铵水溶液(pH=3.7)为流动相,梯度洗脱,采用多反应监测(MRM)模式检测。在优化的条件下,百草枯和敌草快的质量浓度分别在1.0~150μg/L和0.5~75μg/L范围内与色谱峰面积线性相关,相关系数分别为0.997和0.998,检出限分别为0.2、0.1μg/L。百草枯和敌草快加标回收率分别为100.9%、100.8%,测定结果的相对标准偏差分别为2.6%、1.6%(n=6)。该方法适用于尿液中百草枯和敌草快的同时测定。

A method for the simultaneous determination of Paraquat and Diquat in urine by hydrophilic interaction ultra high performance liquid chromatography-tandem mass spectrometry was established. The sample was extracted by phosphate buffer solution(pH=6.8), and purified by a weak cation exchange solid phase extraction column. Waters HILIC column(100 mm×2.1 mm, 1.7 μm) was selected as the separation column, acetonitrile-200 mmol/L ammonium formate aqueous solution(pH=3.7) as the mobile phase, gradient elution, and multi reaction monitoring(MRM) mode was used for detection. Under the optimized experimental conditions, the mass concentrations of Paraquat and Diquat had a good linear relationship with the chromatographic peak area in the range of 1.0-150 μg/L and 0.5-75 μg/L, respectively, the correlation coefficient were 0.997, 0.998, and the detection limits were 0.2, 0.1 μg/L, respectively. The recoveries of Paraquat and Diquat were 100.9% and 100.8%, respectively. The relative standard deviations of the determination results were 2.6% and 1.6%(n=6). The method is suitable for the simultaneous determination of Paraquat and Diquat in urine.