QuEChERS/超高效液相色谱-串联质谱测定人全血中24种磺酰脲类除草剂

Determination of 24 sulfonylurea herbicides in human blood by QuEChERS-UPLC-MS/MS

建立了QuEChERS/超高效液相色谱-串联质谱测定人全血中24种磺酰脲类除草剂的方法。对QuEChERS方法进行优化,样品加入NaCl和无水Na_(2)SO_(4)并取上层清液经Simple-QuEChERS Nano净化柱净化。采用EclipsePlus C18 RRHD色谱柱分离,以乙腈-水(含0.1‰甲酸)为流动相进行梯度洗脱,在多反应监测(MRM)模式下进行检测,内标法定量。在各自线性范围内,24种磺酰脲类除草剂线性关系良好(r> 0.995);检出限为0.1~0.2 ng/mL,定量限为0.2~0.5 ng/mL。加标回收率为93.4%~112.3%,日内相对标准偏差(RSD)为0.6%~8.1%,日间RSD为3.3%~9.7%。方法已用于实际案例中磺酰脲类除草剂的检测。

A QuEChERS-UPLC-MS/MS method was established for the detection of 24 sulfonylurea herbicides in human blood.The sample was extracted with acetonitrile,then NaCl and anhydrous Na_(2)SO_(4) were added into the obtained supernatant,accompanied by purification with Simple-QuEChERS Nano column.Sulfonylurea herbicides were separated on a EclipsePlus C18 RRHD column with acetonitrile and water(containing 0.1‰ formic acid)as mobile phase for gradient elution.The detection was carried out under multiple reaction monitoring(MRM)mode and quantification was conducted by internal standard method.The results showed that the linear ranges of 24 sulfonylurea herbicides were 0.5-100 ng/mL(r > 0.995);the limits of detection were 0.1-0.2 ng/mL,and the limits of quantification were 0.2-0.5 ng/mL.The recoveries were 93.4%-112.3%,the intra-day relative standard deviations(RSDs)were 0.6%-8.1%,and the inter-day RSDs were 3.3%-9.7%.The method has been applied in practical cases for the detection of sulfonylurea herbicides.