基质全溶解-固相萃取-UPLC-MS/MS法分析聚酯纤维中阻燃剂  

Matrix total dissolution concatenated solid phase extraction for determination of phthalate esters in polyester fibers prior to UPLC-MS/MS

作　　者：张梦丹 李盈盈 张思佳 李琳[1] 侯晓虹[2] ZHANG Mengdan;LI Yingying;ZHANG Sijia;LI Lin;HOU Xiaohong(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;School of Pharmaceutical Engineering,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016 [2]沈阳药科大学制药工程学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2024年第9期1254-1262,共9页Journal of Shenyang Pharmaceutical University

摘　　要：目的探索聚酯纤维中常见有机磷酸酯阻燃剂(磷酸三苯酯和三苯基氧化膦)的分析方法。方法通过完全溶解法将样品基质溶解,再采用商品化固相萃取柱PEP-2对提取的样品溶液进行进一步净化,结合UPLC-MS/MS技术测定5种聚酯纤维样品中的两种有机磷酸酯阻燃剂。结果在最优的条件下,建立的分析方法线性关系良好(r≥0.9958),灵敏度高,磷酸三苯酯和三苯基氧化膦方法检测限分别为0.08 ng·g^(-1)和0.014 ng·g^(-1),加标回收率范围为80.2%~104.6%,方法精密度RSD值低于8.8%。结论建立的分析方法准确度高、精密度好、无基质干扰、稳定可靠,为该类基质中痕量污染物的分析提供了新的策略。Objective An analytical method for triphenyl phosphate and triphenylphosphine oxide in polyester fibers was explored.Methods The sample matrix was dissolved by the complete dissolution method,and then the extracted sample solution was further cleaned up using a commercial solid-phase extraction column PEP-2.UPLC-MS/MS technique was used for the determination of two organophosphate flame retardants in five polyester fiber samples.Results Under the optimized conditions,satisfactory linearity was achieved with the correlation coefficient(r)greater than 0.9958,and the sensitivity of the method was high.The method limits of detection of triphenyl phosphate and triphenylphosphine oxide were 0.08 ng·g^(-1)and 0.014 ng·g^(-1),respectively.The spiked recoveries of triphenyl phosphate and triphenylphosphine oxide ranged from 80.2%to 104.6%,and the RSD of method precision was less than 8.8%.Conclusion The above results indicated that the established analytical method was precise,accurate,without matrix interference,reliable and stable,providing a novel strategy for the analysis of trace contaminants in this type of matrix.

关 键 词：聚酯纤维 有机磷酸酯阻燃剂 样品前处理 基质完全溶解法 固相萃取 UPLC-MS/MS 

分 类 号：R917[医药卫生—药物分析学]