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目的:建立大鼠血浆中百草枯HPLC检测方法,为百草枯中毒患者治疗、预后提供试验依据。方法:样品处理采用35%高氯酸(v/v)沉淀蛋白质。DiamonsilTM C18(250mm×4.6mm,5μm)色谱柱,流动相为0.1mol·L-1磷酸缓冲液(含75mmol·L-1庚烷磺酸钠)-乙腈(88∶12),用三乙胺调pH至3.0,检测波长为258nm。结果:所建立方法在20～5000ng·mL-1范围内线性良好,方法平均回收率为87.5%,日内变异RSD小于10%。大鼠灌胃给50mg·kg-1后8h血浆百草枯浓度为(360.3±130.9)ng·mL-1,至第3d则不能检出。结论:该法准确、灵敏、快速,复杂生物基质中杂质无干扰,适用于血浆中百草枯的分析测定。
OBJECTIVE: To establish a HPLC method for the determination of paraquat in rat plasma and provide the experimental basis for the treatment and prognosis of paraquat poisoning patients. Method: The sample was processed for protein precipitation using 35% perchloric acid (v / v). DiamonsilTM C18 (250mm × 4.6mm, 5μm) was used as the mobile phase. The mobile phase consisted of 0.1mol·L-1 phosphate buffer (containing 75mmol·L -1 sodium heptane sulfonate) -acetonitrile (88:12) Adjust pH to 3.0, detection wavelength of 258nm. Results: The established method was linear in the range of 20 ~ 5000 ng · mL-1. The average recovery was 87.5%. The intra-day variation RSD was less than 10%. The plasma paraquat concentration was (360.3 ± 130.9) ng · mL-1 at 8 h after intragastric administration of 50 mg · kg-1, but could not be detected by the third day. Conclusion: This method is accurate, sensitive, rapid, complex non-interference of impurities in biological matrix, suitable for the analysis of paraquat in plasma.