超高效液相色谱法测定儿童指画印泥中柚皮苷和苯甲酸地那铵

UHPLC Determination of Naringin and Denatonium Benzoate in Children′s Finger Paint Pads

儿童指画印泥样品用甲醇与0.02mol·L^-1磷酸二氢钾溶液以体积比3∶7组成的混合液超声萃取20min,冷却至室温,于16 000r·min^-1转速下离心15min,取上清液过0.22μm过滤膜过滤,采用超高效液相色谱法测定滤液中柚皮苷和苯甲酸地那铵的含量。以C18色谱柱为分离柱,用乙腈和pH 4.3的0.02mol·L^-1磷酸二氢钾溶液以不同比例混合的溶液为流动相进行梯度洗脱,用二极管阵列检测器测定。柚皮苷和苯甲酸地那铵的质量浓度均在0.1~5.0mg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)依次为0.75,1.15mg·kg^-1。以空白样品为基体进行加标回收试验,所得回收率为73.5%~104%,测定值的相对标准偏差(n=6)为4.2%~6.6%。

The sample of children′s finger paint pad was extracted ultrasonically for 20 min with a mixture of methanol and 0.02 mol·L-1 KH2PO4 solution(volume ratio,3∶7).After cooling to room temperature,the solution was centrifugated for 15 min at the speed of 16 000 r·min-1.The supernatant was taken and filtered on0.22μm filtering membrane.UHPLC was applied to the determination of naringin and denatonium benzoate in the filtrate.C18 chromatographic column was used as separation column with mixtures of acetonitrile and 0.02 mol·L-1 KH2PO4 solution(pH 4.3)with different mixing ratios as mobile phase in the gradient elution,and diode array detector was adopted for determination.Linear relationships between values of peak area and mass concentration of naringin and denatonium benzoate were kept in the same range of 0.1-5.0 mg·L-1,with detection limits(3 S/N)of 0.75,1.15 mg·kg-1 respectively.On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 73.5%-104%,with RSDs(n=6)of determined values in the range of 4.2%-6.6%.