UPLC法检测明胶空心胶囊中9种合成着色剂

Simultaneous detection of 9 synthetic pigments in vacant gelatin capsules by UPLC

目的:建立UPLC法检测明胶胶囊壳中柠檬黄、新红、苋菜红、胭脂红、日落黄、诱惑红、偶氮玉红、亮蓝、赤藓红9种合成着色剂。方法:样品水溶液经甲醇沉淀,上清液水浴蒸干后,定容过滤,采用UPLC法进行检测。色谱条件:使用BEH C18色谱柱(2.1 mm×50 mm,1.7μm),以10 mmol·L^(-1)乙酸铵为流动相A,甲醇为流动相B,梯度洗脱,流速0.3 m L·min^(-1),柱温30℃,检测波长254 nm。结果:9种合成色素质量浓度在1.0~100.0μg·mL^(-1)范围内均有良好的线性关系,回归系数r>0.998,检出下限为0.10~0.50μg·mL^(-1),回收率为95.1%~101.9%(n=9)。对10批样品中合成着色剂进行检测,结果分别为柠檬黄0.289~0.672 mg·g^(-1),苋菜红0.325 mg·g-1,胭脂红0.282~0.373 mg·g-1,亮蓝0.072~0.226 mg·g-1,其他合成着色剂均未检出。结论:经方法学验证,本法可用于明胶胶囊壳中合成着色剂的检测。

Objective：To establish a UPLC method for simultaneous detection of 9 synthetic pigments,including tartrazine,new red,amaranth,carmine,sunset yellow,fancy red,azorubine pigment,brilliant blue,erythrosine,in vacant gelatin capsules. Methods：Sample solution was prepared with following steps：first it was precipitated by methanol,and then the supernatant was dried with water bath,diluted by mobile phase and filtrated. UPLC analysis was performed on a BEH C18 column（2.1 mm×50 mm,1.7 μm）. The mobile phases with gradient elution were 10 mmol·L-1 ammonium acetate and methanol. The flow rate was set at 0.3 m L·min-1 and the column temperature was controlled at 30 ℃. The sample solution was detected at 254 nm. Results：The liner range of 9 synthetic pigments were between 1.0-100.0 μg·mL-1（r〉0.998）,and the LOD was in the range of 0.10-0.50 μg·mL-1. The average recoveries（n=9）were 95.1%-101.9%. The synthetic pigments contents of ten batches of sample were 0.289-0.672 mg·g-1（tartrazine）,0.325 mg·g-1（amaranth）,0.282-0.373 mg·g-1（carmine）,0.072-0.226 mg·g-1（brilliant blue）,and other synthetic pigments were not detected. Conclusion：The established method is proved by methodology validation which can be used for the detection of synthetic pigments in vacant gelatin capsules.