超声萃取-高效液相色谱法测定棉织物中5种荧光增白剂

HPLC Determination of 5 Fluorescent Whitenings in Cotton Fabric with Ultrasonic Extraction

应用超声萃取-高效液相色谱法测定棉织物中5种荧光增白剂的含量。棉织物样品在40℃温度下用二甲基甲酰胺-水(70+30)混合液超声提取20min。提取液按仪器工作条件进行色谱测定。分离中用Agilent Eclipse XDB-C18色谱柱为固定相,用乙腈和10mmol·L-1乙酸铵溶液以不同比例混合后作为流动相进行梯度洗脱。用二极管阵列检测器测定。5种荧光增白剂的质量浓度均在0.5~200.0mg·L-1范围内与其峰面积呈线性关系。方法的检出限(3S/N)在0.05~0.10mg·L-1之间,测定下限(10S/N)在1.2~2.1mg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在76.5%~103%之间,相对标准偏差(n=6)在2.6%~7.1%之间。

HPLC was applied to the determination of 5fluorescent whitenings in cotton fabric with ultrasonic extraction of sample.The sample was extracted ultrasonically with DMF-H2O(70+30)mixture for 20 min at40 ℃,and the extract was separated on Agilent Eclipse XDB-C18 chromatographic column with mixtures of acetonitile and 10 mmol·L-1 ammonium acetate solution with different ratios as mobile phase in the gradient elution,and detected with DAD.Linear relationships between values of peak area and mass concentration of the 5fluorescent whitenings were kept in the same range of 0.5-200.0mg·L-1,with detection limits(3S/N)in the range of 0.05-0.10mg·L-1 and lower limits of determination(10S/N)in the range of 1.2-2.1mg·kg-1.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 76.5%-103%,with RSD′s(n=6)in the range of 2.6%-7.1%.