摘要
目的建立HPLC法检测明胶空心胶囊中柠檬黄、新红、苋菜红、诱惑红、胭脂红和日落黄6种偶氮类人工合成色素。方法样品水溶液经甲醇沉淀,上清液水浴蒸干,定容过滤,采用HPLC法进行检测。使用色谱柱Waters XBridge C18(4.6 mm×250 mm,5μm),以10 mmol·L^-1醋酸铵为流动相A,甲醇为流动相B,进行梯度洗脱,柱温30℃,进样量10μL,检测波长:柠檬黄为440 nm,新红、苋菜红与诱惑红为520 nm,胭脂红与日落黄为490 nm。结果 6种人工合成色素在9.856~985.6μg·mL^-1(柠横黄)、9.612~961.2μg·mL^-1(新红)、8.539~853.9μg·mL^-1(苋菜红)、9.124~912.4μg·mL^-1(诱惑红)、10.300~1030.0μg·mL^-1(胭脂红)、9.472~947.2μg·mL^-1(日落黄)内与峰面积线性关系良好,检出限为0.90~2.85 mg·kg^-1,回收率为93.3%~100.5%(n=3),RSD为1.2%~3.0%。结论本法可用于明胶空心胶囊中人工合成色素的检测。
Objective To determine 6 azo synthetic pigments, including tartrazine, new red, amaranth, allura red, neucoccin, sunset yellow in vacant gelatin capsules by HPLC. Methods Sample solutions were precipitated by methanol, and the supernatant was dried with water bath, and diluted by water before filtration. HPLC analysis was performed on a Waters XBridge C18 column(4.6 mm×250 mm, 5 μm). The mobile phase with gradient elution was 10 mmol·L^-1 ammonium acetate and methanol. The flow rate was 1.0 mL·min^-1, and the column temperature was controlled at 30 ℃. The sample solution was detected at 440 nm(tartrazine), 520 nm(new red, amaranth and allura red) and 490 nm(neucoccin and sunset yellow). Results The linear range of the 6 azo synthetic pigments was 9.856-985.6 μg·mL-1(tartrazine), 9.612-961.2 μg·mL^-1(new red), 8.539-853.9 μg·mL^-1(amaranth), 9.124-912.4 μg·mL^-1(allura red), 10.300-1030.0 μg·mL^-1(neucoccin), and 9.472-947.2 μg·mL^-1(sunset yellow). The LOD was at 0.90-2.85 mg·kg^-1. The average recovery(n= 3) was at 93.3%-100.5%, with RSDs 1.2%-3.0%. Conclusion The established method can detect azo synthetic pigments in vacant gelatin capsules.
作者
张恒斌
ZHANG Heng-bin(Linyi Inspection and Testing Center,Linyi Shandong 276000)
出处
《中南药学》
CAS
2019年第9期1522-1525,共4页
Central South Pharmacy
