色谱2026，Vol.44Issue(6)：682-693,12.DOI:10.3724/SP.J.1123.2025.09019
超高效液相色谱-串联质谱法测定人体全血中22种有机磷酸酯及其代谢物和11种邻苯二甲酸酯类代谢物
Determination of 22 organophosphates and their metabolites and 11 phthalate metabolites in human whole blood by ultra performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
Organic phosphate esters(OPEs)and phthalate esters(PAEs)are two classes of synthetic compounds widely incorporated into various industrial and consumer products as flame retardants and plasticizers.Both exhibit multi-organ cumulative toxicity.In this study,an ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was de-veloped for the determination of 22 OPEs and their diester metabolites(mOPEs)and 11 phthalate ester metabolites(mPAEs)in whole blood.The whole blood samples were extracted with 0.1%formic acid-acetonitrile by liquid-liquid extraction for protein precipitation,and then purified by HMR S-micro BIO 96-well solid phase extraction column.The filtrate was blown to near dryness with nitrogen,and reconstituted with 0.1%formic acid-acetonitrile solution.The target compounds were detected by UPLC-MS/MS.A Ghost Trap DS-HP chromatographic column(30 mm×2.1 mm)was used as the background ghost peak trap column,and an ACQUITY UPLC® BEH C18 chromato-graphic column(150 mm×2.1 mm,1.7 μm)was used as the analytical column.Methanol and 0.5 mmol/L ammonium acetate were used as mobile phase for gradient elution.Electrospray ionization(ESI)was used for MS detection,with both positive and negative ion scanning in the multiple reaction monitoring(MRM)mode.Isotope internal standard method was used for quantification.The results showed that 33 target compounds could be separated within 15 min,and good linear relationships were observed for all target compounds across their respective mass concentration ranges(r=0.993 3-0.999 8).The limits of detection were 0.003-0.31 ng/mL and the limits of quantification were 0.01-1.02 ng/mL.The spiked recoveries of 33 targets in whole blood samples ranged from 60.5%to 138.3%,with relative standard deviations(RSDs)from 1.6%to 11.0%.The detection rates of tris-(2-chloroisopropyl)phosphate(TCiPP),triphenyl phosphate(TPHP),2-ethylhexyl diphenyl(EHDPP),mono(2-ethyl-5-hydroxyhexyl)phthalate(MEHHP),mono-n-butyl phthalate(MNBP)and mono-n-octyl phthalate(MOP)were 100%in 14 whole blood samples,and the highest detection amount of TPHP was 10.04 ng/mL.The developed method is simple to operate,sensitive,accurate,requires small sample volumes,and is cost-effective on reagents.It is suitable for human biomonitoring,and provides a theoretical basis for monitoring organic phosphate and phthalic ester substances in the population.关键词
有机磷酸酯/邻苯二甲酸酯类代谢物/全血/超高效液相色谱-串联质谱法Key words
organic phosphate esters/phthalate ester metabolites/whole blood/ultra perfor-mance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)分类
化学化工引用本文复制引用
石飞云,徐浩宇,黎俊宏,徐梦媛..超高效液相色谱-串联质谱法测定人体全血中22种有机磷酸酯及其代谢物和11种邻苯二甲酸酯类代谢物[J].色谱,2026,44(6):682-693,12.基金项目
2024年常州市卫生健康委员会青年人才科技项目(QN202463,QN202425) （QN202463,QN202425）
江苏省第六期"333高层次人才培养工程"第三层次培养对象[(2022)3-4-163].Youth Talent Science and Technology Project of Changzhou Municipal Health Commission in 2024(Nos.QN202463,QN202425) （2022）
the Third Level Training Objects of the Sixth"333 High Level Talent Training Project"in Jiangsu Province[(2022)3-4-163]. （2022）
