伪制红薯粉条中非法添加3种合成色素的检测方法

Determination of three synthetic pigments illegally added into sweet potato by HPLC-DAD and HPLC-MS/MS

建立了二极管阵列高效液相色谱法(HPLC-DAD)及高效液相色谱-串联质谱法(HPLC-MS/MS)测定伪制红薯粉条中非法添加人工合成色素柠檬黄、日落黄、亮蓝的检测方法。样品经粉碎后加0.25 mL氨水(氨水和水体积比为1∶1)、50 mL水涡旋2 min,超声20 min,加水定容后进行检测。结果表明:3种合成色素在添加浓度范围均有良好的线性关系,HPLC-DAD的相关系数(R2)为0.999 2~0.999 3,HPLC-MS/MS的相关系数(R2)为0.996 1~0.997 9,HPLC-DAD和HPLC-MS/MS的检出低限分别为0.08~0.3 mg/kg和0.02~0.05 mg/kg,在低、中、高3个水平进行加标回收实验,HPLC-DAD和HPLC-MS/MS回收率分别为83.5%~89.9%和84.2%~92.5%,相对标准偏差分别为0.62%~4.10%和0.96%~4.92%。方法准确、灵敏度高、回收率高,适用于伪制红薯粉条中非法添加合成色素的检测。

Two methods, high-performance liquid chromatography with diode array detector （HPLC-DAD） and high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） were developed for the determina- tion of synthetic pigments such as tartrazine, sunset yellow, brilliant blue which were illegally added into sweet potato noodles. The crushed samples were extracted by ultrasound for 20 min and vortex blending assisted extraction 2 min in 0.25 mL ammonia solution （1： 1, v/v）. The HPLC-DAD and HPLC-MS/MS methods were used. The calibration curves of each synthetic pigment showed good linear relationships. The Square correlation coefficients of all pigments were from 0. 999 2 - 0. 999 3 by HPLC-DAD and from 0. 996 1 - 0.997 9 by HPLC-MS/MS. The determination limits of 3 synthet- ic pigments were 0.08 -0.3 mg/kg by HPLC-DAD and 0.02 -0.05 mg/kg by HPLC-MS/MS. The recovery tests were performed at the low, middle and high level with mixed standard solution of 3 synthetic pigments. The recoveries of HPLC-DAD and HPLC-MS/MS were 83.5% - 89.9% and 84.2% - 92.5% respectively. Meanwhile, the relative standard deviations of HPLC-DAD and HPLC-MS,/MS were 0.62% -4. 10% and 0.96% -4.92% respectively. The method of HPLC-DAD and HPLC-MS/MS were accurate, sensitive and accurate for validation of positive samples.