论文部分内容阅读
目的建立血浆中毒死蜱(CPF)及其主要代谢物3,5,6-三氯-2-吡啶醇(TCP)的超高效液相色谱(UPLC)测定方法。方法取0.50 m L待测血浆经乙酸乙酯萃取,氮气吹干,乙腈定容,采用C18柱分离,以乙腈∶水为流动相梯度洗脱,在二极管阵列检测器检测波长为298 nm(0.0~2.0 min)和289 nm(2.0~5.0 min)的紫外光谱下,经UPLC仪测定。结果 CPF和TCP在质量浓度为1.00~50.00 mg/L时线性关系良好,相关系数均为0.999 9,检出限均为0.30 mg/L,定量限均为1.00 mg/L。加标回收率分别为87.20%~103.08%和86.20%~99.28%,批内相对标准偏差(RSD)分别为5.28%~6.17%和2.32%~4.43%,批间RSD分别为6.62%~7.53%和3.55%~5.24%。样品在4℃冰箱内可保存7 d。结论本方法准确可靠,简便实用,可用于测定血浆中CPF和TCP。
Objective To establish a method for the determination of chlorpyrifos (CPF) in plasma and its metabolite 3,5,6-trichloro-2-pyridinol (TCP) by ultra performance liquid chromatography (UPLC). Methods The plasma samples were extracted with ethyl acetate (0.50 m L), dried under nitrogen, diluted with acetonitrile and eluted with a C18 column. The mobile phase consisted of acetonitrile and water as eluent, and the detection wavelength was 298 nm (0.0 ~ 2.0 min) and 289 nm (2.0 ~ 5.0 min) by UV spectroscopy. Results The linearity of CPF and TCP was good at the mass concentration of 1.00-50.00 mg / L with the correlation coefficients of 0.999 9 and the detection limits of 0.30 mg / L and the limits of quantification of 1.00 mg / L. The recoveries of spiked samples ranged from 87.20% to 103.08% and from 86.20% to 99.28%, respectively. The relative standard deviations (RSDs) in batches ranged from 5.28% to 6.17% and 2.32% to 4.43%, respectively, and the RSDs were 6.62% to 7.53% And 3.55% -5.24%. Samples can be stored in a 4 ℃ refrigerator for 7 days. Conclusion The method is accurate and reliable, simple and practical, and can be used for the determination of CPF and TCP in plasma.