超高效液相色谱-串联质谱法测定血液中噻螨酮

Determination of hexythiazox in blood by UPLC-MS/MS

目的建立血液中噻螨酮的超高效液相色谱-质谱检测方法。方法采用乙腈沉淀蛋白法进行样本前处理,使用Acquity UPLCHSS T3（50mm×2.1mm,1.8μm）色谱柱,乙腈-0.1%甲酸梯度洗脱,电喷雾多反应监测模式（MRM）检测。结果血液中噻螨酮具有良好的色谱峰,无内源性物质干扰,在0.1-500.0ng/m L范围内线性良好,R2=0.998 7,回收率80.5%-92.8%,最低检出限0.02ng/m L,日内精密度3.5%-6.9%,日间精密度8.3%-11.2%。结论本文建立的超高效液相色谱-质谱检测法操作简便快速,提取回收率高,灵敏度高,重现性好,可用于实际案例中噻螨酮的检测。

Objective This study establishes an analytical method to detect hexythiazox in blood by via the Acquity UPLC HSS T3 （50mm × 2. 1mm, 1.8 μm ） column using acetonitrile -0. 1% formic acid gradient elution. The detection was taken under electrospray ionization and multiple reaction monitoring mode （MRM）. Results This method can produce good chromatographic peaks for the hexythiazox in blood, without endogenous substances interference. In the range of 0. 1 - 500. 0ng/mL, the data show good linearity, with R2 =0. 998 7. The recovery rate is 80.5% -92. 8%. The detection limit is 0.02ng/mL. The inter-day precision and intra-day precision are 3.5% -6.9% and 8.3% - 11.2% , respectively. Conclusion The method is simple and rapid, high extraction recovery, high sensitivity, good reproducibility, which can be used for the detection of hexythiazox in the actual case.