QuEChERS/超高效液相色谱法测定水性涂料中5种酚和酚类衍生物

Determination of Five Phenolic Compounds in Waterborne Coatings by QuEChERS/Ultra High Performance Liquid Chromatography

建立了水性涂料中5种酚和酚类衍生物（双酚A、辛基酚、壬基酚、辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚）含量的QuEChERS净化、超高效液相色谱/荧光测定的分析方法.样品先加入QuEChERS（PSA＋C18＋ MgSO4）,充分涡旋分散,脱水除杂后,加入二氯甲烷-乙腈（1：3）提取,采用Waters UPLC BEH C18色谱柱,以乙腈-水为流动相进行梯度洗脱分离提取液,荧光检测器检测,外标法定量.在优化实验条件下,5种化合物的质量浓度在5～1 300μg/L范围内与其峰面积线性关系良好,相关系数均大于0.9995,方法检出下限（MLOD）为0.4～1.0 mg/kg,在加标水平为1.5～35.0 mg/kg时,水性涂料样品中5种待测物的平均加标回收率为97.5％～114％,相对标准偏差（n=6）为2.6％ ～ 6.5％.该法准确、灵敏,适用于水性涂料中5种酚和酚类衍生物含量的快速分析.

A method was developed for the simultaneous determining of five phenolic compounds, in- eluding biphenol A （ BPA）, oetylphenol （ OP）, nonylphenol （ NP）, oetyl phenoxypoly （ethyleneoxy） ethanol （ OPEO ） and nonylphenoxypoly （ ethyleneoxy ） ethanol （ NPEO ） ） in waterborne coatings by QuEChERS/ultra high performance liquid chromatography with fluorescence detector（UPLC/FLD）. Samples were dispersed firstly by QuEChERS（ PSA ＋ C18 ＋ MgSO4 ） , and stirred uniformly to reduce the impurity, then extracted ultrasonically with diehloromethane - acetonitrile （ 1 ： 3 ）. The ultimate solution was quantified by UPLC/FLD on a Cls column by gradient elution with water- acetonitrile as mobile phase at a flow rate of 0. 2 mL/min. Under the optimized conditions, the method had good linear relationships （ r 〉 0. 999 5 ） in the range of 5 - 1 300 μg/L for five compounds. The method de- tection limits（MLOD） for targeted compounds ranged from 0. 4 mg/kg to 1.0 mg/kg. The spiked re- coveries of five compounds varied from 97.5% to 114% with relative standard deviations （RSDs） of 2. 6% -6. 5%. The results showed that the method was simple, sensitive and precise, and could meet the qualification and quantification analysis requirements for BPA, OP, NP, OPEO and NPEO residues in waterborne coatings.