超声萃取液相色谱法测定纺织品中的仿雌激素

Determination of Xenoestrogens in Textiles by High Performance Liquid Chromatography with Ultrasound Extraction

本文采用超声萃取前处理技术、高效液相色谱法建立了一种同时测定纺织品中5种仿雌激素的检测方法。样品以乙腈为萃取剂进行超声萃取,探讨了超声波萃取最佳工艺条件,在最优超声萃取条件下,以仿雌激素的色谱峰面积(Y)对浓度(X)进行线性拟合,测试各仿雌激素拟合曲线相关系数及不同基质平均回收率和精密度,并应用于实际样品的测试分析。结果表明,5种仿雌激素在0.1~50.0 mg/L呈良好的线性关系,相关系数均大于0.999;方法定量限(S/N=10)0.2~0.8 mg/kg;添加水平为0.5~10.0 mg/kg时,测得回收率为87.2%~101.3%,相对标准偏差(RSD,n=6)为1.3%~4.8%。该方法具有前处理简便、回收率高、精密度好等优点,适用于测定纺织品中仿雌激素。

In this paper,A novel method was established to determine five xenoestrogens in textiles by high performance liquid chromatography-fluorescence detection combined with Ultrasound extraction(UA-HPLC-FLD).The sample was subjected to ultrasonic extraction with acetonitrile as the extraction agent,the optimal ultrasonic extraction process conditions were discussed.Under the optimal ultrasonic extraction conditions,a linear fit was performed on the concentration(X)with the chromatographic peak area(Y)of xenoestrogens,and it tested the correlation coefficient of each xenoestrogens fitting curve and the average recovery and precision of different matrices,which were applied to the analysis of actual samples.The results show that the five xenoestrogens have a good linear relationship in the range of 0.1~50.0 mg/L,and correlation coefficients are larger than 0.999.The method limits of quantification(MLOQ)are from 0.2 mg/kg to 0.8 mg/kg(S/N=10).When the addition level is from 0.5~10.0 mg/kg,the recoveries rate is 87.2%~101.3%,and the relative standard deviation is 1.3%~4.8%.The method has the advantages of convenient pre-processing,recoveries rate is higher and precise,which is suitable to be used to measure the xenoestrogens in textiles.