论文部分内容阅读
目的建立人血浆中百草枯的高效液相色谱快速测定方法。方法用正交试验优化色谱条件,流动相为甲醇-缓冲液(10:90,v/v),缓冲液为20 mmol/L的十二烷基庚烷磺酸钠(含20 mmol/L磷酸,用三乙胺调节p H为3.5),检测波长:256 nm,流速:0.80 ml/min,柱温为室温。样品依次用乙腈、二氯甲烷处理沉淀血浆中蛋白质并除去脂溶性杂质,取20μl上清液进样测定。结果血浆百草枯在0.1μg/ml到10μg/ml范围内线性关系良好,回归方程为y=6442.6x+44.47(r=0.9992),平均回收率为93.8%-101.1%,日内RSD为3.08%,日间RSD为3.92%。结论该方法简便快速、准确灵敏,适用于人血浆中百草枯快速检测,为百草枯中毒患者的临床诊断提供参考依据。
Objective To establish a method for rapid determination of paraquat in human plasma by high performance liquid chromatography. Methods The orthogonal test was used to optimize the chromatographic conditions. The mobile phase was methanol-buffer (10:90, v / v) and the buffer was 20 mmol / L sodium dodecylheptane sulfonate (containing 20 mmol / L phosphoric acid , Adjusted to pH 3.5 with triethylamine), detection wavelength: 256 nm, flow rate: 0.80 ml / min, column temperature at room temperature. Samples were treated sequentially with acetonitrile and methylene chloride to remove precipitated plasma proteins and remove lipid-soluble impurities, and 20 μl of supernatant was injected into the sample. Results The linearity of plasma paraquat in the range of 0.1μg / ml to 10μg / ml was good, the regression equation was y = 6442.6x + 44.47 (r = 0.9992), the average recovery was 93.8% -101.1%, the intraday RSD was 3.08% The day RSD was 3.92%. Conclusion The method is rapid, sensitive and accurate. It is suitable for rapid detection of paraquat in human plasma and provides a reference for the clinical diagnosis of paraquat poisoning.