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目的:建立HPLC法测定人血清中百草枯含量。方法:色谱柱:Kromasil C_(18)柱(200 mm×4.6 mm,5μm),流动相:乙腈-水(含0.03 mol·L~(-1)庚烷磺酸钠,0.24 mol·L~(-1)磷酸)=3∶97(用三乙胺调pH至2.0);检测波长258 nm;柱温25℃;进样体积20μl;流速0.8 ml·min~(-1)。结果:百草枯在0.106~10.6 mg·L~(-1)浓度范围内线性关系良好(r=0.999 3),最低检出浓度为0.065 mg·L~(-1)。高、中、低3种浓度样品绝对回收率>89.4%,方法回收率>94.4%,日内精密度RSD在0.12%~1.74%之间,日间精密度RSD在0.44%~2.89%之间。结论:该方法操作简便易行、灵敏度高、专属性强,适用于百草枯的人体血清浓度测定。
Objective: To establish a HPLC method for the determination of paraquat in human serum. Methods: Kromasil C 18 column (200 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of acetonitrile-water containing 0.03 mol·L -1 sodium heptane sulfonate and 0.24 mol·L ~ -1) phosphoric acid) = 3:97 (pH adjusted to 2.0 with triethylamine); detection wavelength was 258 nm; column temperature was 25 ℃; injection volume was 20μl; flow rate was 0.8 ml · min -1. Results: Paraquat had a good linearity (r = 0.999 3) at a concentration range of 0.106-10.6 mg · L -1, with a minimum detectable concentration of 0.065 mg · L -1. The absolute recovery of high, medium and low concentration samples was> 89.4%, the recovery rate was> 94.4%. The intraday RSD ranged from 0.12% to 1.74%. The intraday RSD ranged from 0.44% to 2.89%. Conclusion: The method is simple and easy to operate with high sensitivity and specificity. It is suitable for the determination of paraquat in human serum.