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，1.7 μm），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 mL·min-1，柱温30℃，检测波长254 nm。结果：9种合成色素质量浓度在1.0~100.0 μg·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0.10~0.50 μg·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 mL·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.
