建立一种快速检测病人血清中百草枯浓度的方法。本文采用乙腈沉淀血液中蛋白,色谱柱为岛津vp-ODS柱,以乙腈-0.02 mol/L辛烷基磺酸钠(4∶6)为流动相,流速1.0 mL/min,PDA检测器,检测波长为258 nm,柱温25℃。结果是在0.1-100μg/mL范围内线性关系良好(r=0.999 3);回收率为94.87%-105.51%;精密度RSD值为3.08%,重复性RSD值为2.26%。以该色谱条件对某患者的血清进行检测,外标法计算得血清中百草枯浓度为5.91μg/mL。实验证明本方法蛋白沉淀完全,没有杂质峰干扰,出峰时间较早,灵敏度高,可快速检测病人血清中百草枯浓度,为临床治疗提供参考。
To establish a rapid method for the determination of paraquat in patient's serum, this analysis used acetonitrile to precipitate protein in the blood and conducted on a vp-ODS column. The mobile phase consists of acetonitrile - 0.02 mol/L symplectic alkyl sulfonate (4: 6), and the flow rate is 1.0 mL/min. The analysis used PDA detector, and the detection wavelength was 258 nm and the column temperature was 25 ℃. The results were a good linearity in the rage of 0.1-100 μg/mL (r = 0.999 3); The recovery ratio was 94.87%-105.51%; Precision RSD value was 3.08%, the repeatability RSD value was 2.26%. In the chromatographic conditions for some of patient's serum detection, the external standard method for calculating the concentration of serum paraquat was 5.91 μg/mL. Conclusions: The method of protein precipitate is complete, without impurity peak, with an earlier peak time and high sensitivity, which can quickly detect patients with paraquat concentration in serum, and provide reference for clinical treatment.