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目的建立一种灵敏、准确测定血浆中毒死蜱(chlorpyrifos,CPF)及其主要代谢物3,5,6-三氯-2-吡啶醇(3,5,6-trichloro-2-pyridinol,TCP)的气相色谱(GC)方法。方法取0.5 m L家兔血浆加入乙酸乙酯进行液液萃取,离心后取上层有机相,氮气40℃吹干,残留物加入乙酸乙酯定容后,再加入N-甲基叔丁基二甲基硅基三氟乙酰胺(MTBSTFA),50℃下对TCP进行衍生1 h。样品采用气相色谱仪进行检测,以HP-5毛细管柱分离,电子捕获检测器检测。以待测物质的保留时间定性,外标法峰面积定量。结果 CPF和TCP在8 min内得到良好分离。CPF和TCP的质量浓度在0.01~2.50 mg/L的线性范围内与峰面积相关性良好,相关系数分别为0.999 7和0.999 8;最低检测限均为1μg/L;精密度RSD均小于10%;加标回收率分别为77.60%~106.16%和72.00%~99.86%。结论此方法灵敏准确,简便可靠,可用于血浆中CPF与TCP的含量分析。
Objective To establish a sensitive and accurate method for the determination of chlorpyrifos (CPF) and its major metabolite 3,5,6-trichloro-2-pyridinol (TCP) Gas chromatography (GC) method. Methods 0.5 ml rabbit plasma was added with ethyl acetate for liquid-liquid extraction. After centrifugation, the upper organic phase was taken and dried under nitrogen at 40 ° C. The residue was added with ethyl acetate and the volume was increased. N-methyl tert-butyldi Methylsilyl trifluoroacetamide (MTBSTFA) was used to derive TCP at 50 ° C for 1 h. The samples were detected by gas chromatography, separated by HP-5 capillary column and detected by electron capture detector. To be tested substance retention time qualitative external standard peak area quantitative. Results CPF and TCP were well separated within 8 min. The correlation coefficient between the concentration of CPF and TCP in the linear range of 0.01-2.50 mg / L was 0.999 7 and 0.999 8, respectively, and the lowest detection limit was 1 μg / L. The RSDs of precision were less than 10% The spiked recoveries were 77.60% -106.16% and 72.00% -99.86%, respectively. Conclusion This method is sensitive and accurate, simple and reliable, and can be used for the content analysis of CPF and TCP in plasma.