摘要
文章研究一种利用溶剂萃取样品并采用高效液相色谱-静电场轨道阱质谱仪(HPLC-Orbitrap)测定塑料中有机磷酸酯类阻燃剂的方法。使用甲苯和二氯甲烷混合溶剂提取样品,经甲醇沉淀基质离心后,利用C18色谱柱(100.0 mm×2.1 mm,2.6μm)分离。以含体积分数0.1%甲酸的5 mmol/L甲酸铵溶液和甲醇作为流动相,采用数据依赖型扫描(DDA)模式扫描,采用二级质谱离子进行定性分析,采用外标法进行定量分析。有机磷酸酯类阻燃剂在1~200μg/L的质量浓度范围内线性关系良好,相关系数R2大于0.9950。当样品称样量为0.5 g时,检出限为1.03~3.94μg/kg,定量限为4.12~15.80μg/kg。以此方法对46个实际样品进行测试,均测出多种有机磷酸酯类物质,总量为0.08~451.00 mg/kg。该方法操作步骤简单、准确性高、灵敏度低,是一种快速、高效、准确检测有机磷酸酯类阻燃剂的方法。
In this paper,a method for the determination of organic phosphate esters flame retardants in plastics by high performance liquid chromatography-electrostatic field orbitrap mass spectrometry(HPLC-Orbitrap)was studied.Samples were extracted using a mixed solvent of toluene and methylene chloride,centrifuged in a methanol precipitation matrix,and separated by a C18 column(100.0 mm×2.1 mm,2.6μm).A 5 mmol/L ammonium formate solution containing 0.1%volume fraction of formic acid and methanol were used as mobile phases,and the data-dependent scanning(DDA)mode was used to scan,qualitative analysis was performed using tandem mass spectrometry(MS/MS)ions,and quantitative analysis was carried out using the external standard method.Organic phosphate esters flame retardants showed a good linear relationship in the mass concentration range of 1~200μg/L,and the correlation coefficient R2 was larger than 0.9950.When the sample was weighed at 0.5 g,the limit of detection was 1.03~3.94μg/kg,and the limit of quantification was 4.12~15.80μg/kg.In this method,46 actual samples were tested,and a variety of organic phosphate esters were detected,with a total amount of 0.08~451.00 mg/kg.This method is a rapid,efficient and accurate method for the detection of organic phosphate esters flame retardants with simple operation steps,high accuracy and low sensitivity.
作者
熊大伟
王月
李智
刘中贤
李桂晓
贺祥珂
XIONG Dawei;WANG Yue;LI Zhi;LIU Zhongxian;LI Guixiao;HE Xiangke(Shandong Institute for Product Quality Inspection,Jinan 250102,China)
出处
《塑料科技》
北大核心
2025年第9期152-157,共6页
Plastics Science and Technology
基金
山东省市场监督管理局科研项目(sdscjgj2024zj01)。
关键词
电子电气塑料制品
静电场轨道阱质谱
有机磷酸酯
阻燃剂
增塑剂
Electronic and electrical plastic products
Electrostatic field orbitrap mass spectrometry
Organic phosphate esters
Flame retardant
Plasticizer
