阴离子交换固相萃取-高效液相色谱法快速测定中成药中10种合成色素的方法研究
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摘要
目的:建立快速测定中成药中苋菜红、胭脂红、诱惑红、赤藓红、酸性红73、新品红、罗丹明B、苏丹红Ⅰ、808猩红、苏丹红Ⅳ等10种合成色素的高效液相色谱法(HPLC)测定方法。方法:样品用70%乙醇超声提取后,再经阴离子固相去除大部分基质干扰,采用安捷伦C18色谱柱(250 mm×4. 6 mm,5μm);以甲醇-0. 02 mol/L乙酸铵溶液为流动相梯度洗脱,以二极管阵列检测器检测,流速为1. 0 m L/min,检测波长为520 nm,柱温为35℃。结果:以心脑康胶囊为基质,这10种色素在10～100μg/m L范围内线性关系良好,相关系数均在0. 999以上,检测限为1. 05～5. 55μg/m L,回收率为83. 6%～99. 2%(n=9),RSDs为1. 2%～3. 6%。结论:本方法简单可行,结果准确可靠,重复性好,可用于中成药中多种掺伪红色色素的快速检测。
Objective: To establish a high performance liquid chromatography method for rapid determination of 10 kinds of artificial pigments including amaranth,carmine,allura red,erythrosine,brilliant crocein,new fuchsine,rhodamine B,sudanⅠ,scarlet 808,sudan Ⅳ in Chinese patent drug. Methods: The sample were ultrasonic extracted by 70% methanol,then purified by anion exchange solid phase extraction( SPE). A reversed phase column Agilent-C18( 250 mm × 4. 6 mm,5 μm) was used. Taking gradient elution of methanol-0. 02 mol/L ammonium acetate solution as the mobile phase with the application of diode array detector. The flow rate was 1. 0 m L/min,the wavelength for detection was 520 nm,and the column temperature was35 ℃. Results: Ten pigments presented in xinnaokang capsule possessed good linear correlation in the concentration range from10 μg/L to 100 μg/L,their quantitative detection limits ranged from 1. 05 μg/m L to 5. 55 μg/m L and their recoveries ranged from 83. 6% to 99. 2%,the RSDs ranged from 1. 2% to 3. 6%. Conclusion: This method is simple,accurate and reliable,with good reproducity,which can be used for rapid determination of multiple red pigments in Chinese patent drug.
Objective: To establish a high performance liquid chromatography method for rapid determination of 10 kinds of artificial pigments including amaranth,carmine,allura red,erythrosine,brilliant crocein,new fuchsine,rhodamine B,sudanⅠ,scarlet 808,sudan Ⅳ in Chinese patent drug. Methods: The sample were ultrasonic extracted by 70% methanol,then purified by anion exchange solid phase extraction( SPE). A reversed phase column Agilent-C18( 250 mm × 4. 6 mm,5 μm) was used. Taking gradient elution of methanol-0. 02 mol/L ammonium acetate solution as the mobile phase with the application of diode array detector. The flow rate was 1. 0 m L/min,the wavelength for detection was 520 nm,and the column temperature was35 ℃. Results: Ten pigments presented in xinnaokang capsule possessed good linear correlation in the concentration range from10 μg/L to 100 μg/L,their quantitative detection limits ranged from 1. 05 μg/m L to 5. 55 μg/m L and their recoveries ranged from 83. 6% to 99. 2%,the RSDs ranged from 1. 2% to 3. 6%. Conclusion: This method is simple,accurate and reliable,with good reproducity,which can be used for rapid determination of multiple red pigments in Chinese patent drug.
引文
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[5]宋银森,范天黎.中药材中合成色素采用阴离子交换固相萃取HPLC快速测定的效果[J].北方药学,2017,14(8):1-2.
[2]国家食品药品监督管理局.药品检验补充检验方法和检验项目批准件汇编(2003~2008)[S]. 2010:150; 152-160.
[3]蒋玲,饶伟文.中药染色掺假的研究进展[J].首都医药,2011,18(16):16-18.
[4]孙健,冯睿,胡青.等.聚酰胺固相萃取-HPLC法同时测定中药材中16种合成酸性色素[J].中成药.2015,37(5):1031-1135.
[5]宋银森,范天黎.中药材中合成色素采用阴离子交换固相萃取HPLC快速测定的效果[J].北方药学,2017,14(8):1-2.