液相色谱-串联质谱法测定尿液中7种有机磷酸酯代谢物

发布时间：2018-06-23 03:15

  本文选题：液相色谱-串联质谱 + 有机磷酸酯　； 参考：《分析化学》2017年11期

【摘要】：利用液相色谱-三重四极杆质谱(LC-MS/MS)联用技术,建立了人尿液中7种有机磷酸酯代谢产物-有机磷酸二酯的检测方法。针对不同理化性质的有机磷酸二酯,采用固相萃取技术进行富集净化,筛选出高效的固相萃取柱,并对其洗脱条件进行优化;同时,对流动相和质谱参数进行优化,获取用于各代谢产物定性与定量分析的特征离子对。研究结果表明,前处理采用Oasis WAX固相萃取柱富集、2 m L含5%氨水的甲醇和2 m L甲醇洗脱目标物,除磷酸二乙酯(DEP,17.8%~36.2%)外,其余目标化合物回收率均在60.5%~104.0%之间。在优化的液相色谱条件下,7种化合物可达到完全基线分离。7种有机磷酸二酯的检测限和定量限分别在0.005~0.2μg/L和0.02~0.5μg/L之间,日内和日间精密度结果(RSD≤15.4%)表明,本方法具有较好的稳定性和重现性。本方法用于普通人群尿液中有机磷酸二酯的检测,7种化合物在尿液中均有检出,总浓度在0.5~6.7μg/L之间。
[Abstract]:By means of liquid chromatography-quadrupole mass spectrometry (LC-MS / MS), a method for the determination of seven organophosphate metabolites in human urine, organophosphate diester, was developed. For organophosphate diesters with different physical and chemical properties, the solid phase extraction (SPE) technique was used to purify and purify the organophosphate, and the high efficient SPE column was selected, and the elution conditions were optimized, and the mobile phase and mass spectrometry parameters were optimized. The characteristic ion pairs for qualitative and quantitative analysis of metabolites were obtained. The results showed that the recovery rate of the other target compounds was between 60.5% and 104.0% with the exception of diethyl phosphate (DEP17.8%) and methanol elution (36.2%) with the exception of methanol and 2 mL methanol eluting in 2 mL ammonia containing 5% ammonia in the pre-treatment with Oasis WAX solid phase extraction column. The recoveries of the other target compounds were between 60.5% and 104.0%, with the exception of diethyl phosphate (DEP17.8%). Under the optimized liquid chromatography conditions, the detection limits and quantitative limits for the complete baseline separation of 7 organophosphate diesters were within the range of 0.005 渭 g / L and 0.02 渭 g / L, respectively. The results of intra-day and inter-day precision (RSD 鈮，

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