高效液相色谱-紫外检测法快速测定BDP中微量TPP  

Rapid Determination of Trace TPP in BDP by High Performance Liquid Chromatography with Ultraviolet Detection

作　　者：王书奇 李云飞 苑松 王国杰 王一业 WANG Shuqi;LI Yunfei;YUAN Song;WANG Guojie;WANG Yiye(Lihuayi Weiyuan Chemical Co.,Ltd.,Dongying 257400,China)

机构地区：[1]利华益维远化学股份有限公司,山东东营257400

出　　处：《山东化工》2024年第24期121-124,共4页Shandong Chemical Industry

摘　　要：磷酸三苯酯(TPP)作为一种重要的磷系阻燃剂,被广泛应用于各种塑料、橡胶、纤维中。然而,随着毒理研究的深入,人们发现TPP对环境和人体健康都带来严重威胁。相比之下,双酚A-双(二苯基磷酸酯)(BDP)由于具有更大的分子量、良好的耐迁移性、高稳定性、高沸点和低挥发性,成为替代TPP的理想选择。然而,BDP产品中不可避免地含有微量的TPP,这对BDP的阻燃性能和稳定性产生一定影响。因此,需要建立一种准确检测BDP中微量TPP的方法。本研究采用高效液相色谱-紫外检测法快速测定TPP含量,并通过流动相配比、紫外吸收波长和柱温等方面考察了色谱条件对TPP检测的影响,并排除了高黏度BDP对TPP检测的干扰。最优的色谱条件为:使用100%甲醇作为流动相,紫外吸收波长为260 nm,柱温为25℃。在该条件下,配置了5个浓度梯度的TPP标准溶液进行色谱分析,得到了良好的线性关系,相关系数R^(2)=0.9994。本研究的检出限(LOD)和定量限(LOQ)分别为1.28×10^(-4)mg/mL和4.27×10^(-4)mg/mL。在最优色谱条件下,对样品进行加标回收率测试,回收率在80%~96%之间,相对标准偏差RSD在0.03%~0.23%之间,表明方法具有高精密度和良好的重复性。该分析方法还应用于市场上两个样品的TPP含量检测,样品1含量为0.69%,样品2含量为0.58%。目前,有关TPP直接检测的研究报道较多,但对其他磷系阻燃剂中TPP的检测研究较少。本研究以推动环保阻燃剂的应用为目标,贯彻绿色、可持续发展的战略需求,提供了一种环保磷系阻燃剂BDP中微量TPP的分离检测方法。Triphenyl phosphate(TPP)is an important phosphorus-based flame retardant widely used in various plastics,rubber,and fibers.However,with the deepening of toxicological resear,chit has been found that TPP not only contaminates the environment but also poses a serious threat to human health.On the other hand,bisphenol A-bis(diphenyl phosphate)(BDP)has emerged as a promising alternative to TPP due to its larger molecular weight,better migration resistance,higher stability,higher boiling point,and lower volatility.However,BDP products inevitably contain trace amounts of TPP,which can affect the flame retardant performance and stability of BDP.Therefore,it is necessary to establish a reliable detection method for quantifying trace amounts of TPP in BDP.In this study,a rapid determination of TPP content in BDP was carried out using high-performance liquid chromatography with ultraviolet detection.The chromatographic conditions,including mobile phase composition,UV absorption wavelength,and column temperature,were investigated and studied for their effects on TPP detection.The interference of high viscosity BDP on TPP detection was also addressed.The optimized chromatographic conditions were determined as follows:100%methanol as the mobile phase,UV absorption wavelength at 260 nm,and column temperature at 25℃.Under the optimal chromatographic conditions,a series of'TPP standard solutions with five concentration gradients were prepared and analyzed by HPLC.A good linear relationship with a correlation coefficient(R^(2))of 0.9994 was obtained.The limits of detection(LOD)and quantification(LOQ)were determined to be 1.28×10^(-4)mg/mL,and 4.27×10^(-4)mg/mL,respectively.In the best conditions,the spiked recovery rates of TPP in blank samples ranged from 80%to 96%,with relative standard deviations(RSD)between 0.03%and 0.23%,indicating high precision and good repeatability of the method.The developed analytical method was applied to determine the TPP content in two market samples,yielding concentrations(mass fraction)of 0.69

关 键 词：阻燃剂 磷酸三苯酯 双酚A-双(二苯基磷酸酯) 高效液相色谱-紫外检测 

分 类 号：O653[理学—分析化学]