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目的:建立检测人血浆百草枯浓度的高效液相色谱方法。方法:流动相为乙腈-3 mmol·L~(-1) SDS-0.2%TFA(35:28:37),流速为1.0 ml·min~(-1),检测波长258 nm,柱温35℃,内标为卡马西平。用乙腈沉淀血浆蛋白处理后,进行高效液相色谱分析。结果:血浆百草枯在0.5～100.0 mg·L~(-1)范围内线性关系良好(r=0.999 8)。高、中、低三个浓度(1.00,10.00,50.00 mg·L~(-1))的相对回收率分别为(103.06±4.04)%,(100.20±3.00)%和(99.33±2.26)%;日内RSD分别为4.85%,5.97%和4.91%;日间RSD分别为6.60%,5.98%和4.10%。结论:本方法准确可靠,简便快速,适用于百草枯中毒患者的血药浓度检测。
Objective: To establish a method for the determination of paraquat in human plasma by high performance liquid chromatography. Methods: The mobile phase consisted of acetonitrile-3 mmol·L -1 SDS-0.2% TFA (35:28:37), the flow rate was 1.0 ml · min -1, the detection wavelength was set at 258 nm and the column temperature was 35 ℃ , The internal standard is carbamazepine. After plasma protein was precipitated with acetonitrile, high performance liquid chromatography was performed. Results: The plasma paraquat showed a good linear relationship (r = 0.999 8) within the range of 0.5-100.0 mg · L -1. The relative recoveries were (103.06 ± 4.04)%, (100.20 ± 3.00)% and (99.33 ± 2.26)% for high, middle and low concentrations of 1.00, 1.00 and 50.00 mg · L -1, respectively. Intraday RSD were 4.85%, 5.97% and 4.91% respectively; daytime RSD was 6.60%, 5.98% and 4.10% respectively. Conclusion: The method is accurate, reliable, simple and rapid and suitable for the determination of plasma concentration of paraquat poisoning patients.