本文選題：液相色譜-串聯(lián)質(zhì)譜 + 有機磷酸酯　； 參考：《分析化學(xué)》2017年11期

【摘要】：利用液相色譜-三重四極桿質(zhì)譜(LC-MS/MS)聯(lián)用技術(shù),建立了人尿液中7種有機磷酸酯代謝產(chǎn)物-有機磷酸二酯的檢測方法。針對不同理化性質(zhì)的有機磷酸二酯,采用固相萃取技術(shù)進行富集凈化,篩選出高效的固相萃取柱,并對其洗脫條件進行優(yōu)化;同時,對流動相和質(zhì)譜參數(shù)進行優(yōu)化,獲取用于各代謝產(chǎn)物定性與定量分析的特征離子對。研究結(jié)果表明,前處理采用Oasis WAX固相萃取柱富集、2 m L含5%氨水的甲醇和2 m L甲醇洗脫目標(biāo)物,除磷酸二乙酯(DEP,17.8%~36.2%)外,其余目標(biāo)化合物回收率均在60.5%~104.0%之間。在優(yōu)化的液相色譜條件下,7種化合物可達到完全基線分離。7種有機磷酸二酯的檢測限和定量限分別在0.005~0.2μg/L和0.02~0.5μg/L之間,日內(nèi)和日間精密度結(jié)果(RSD≤15.4%)表明,本方法具有較好的穩(wěn)定性和重現(xiàn)性。本方法用于普通人群尿液中有機磷酸二酯的檢測,7種化合物在尿液中均有檢出,總濃度在0.5~6.7μg/L之間。
[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，

本文編號：2055513