摘要
目的:建立红花中酸性橙Ⅱ的高效液相色谱定量测定方法,了解市售中药饮片红花中酸性橙Ⅱ的污染情况。方法:HPLC 法,Diamonsil^(TM) C_(18)色谱柱(250 mm ×4.6 mm,5μm),流动相为0.025 mol·L^(-1)磷酸二氢钾溶液(含0.2%三乙胺,用磷酸调节 pH 值为3.0):乙腈(55:45),检测波长为484 nm,流速为1.0 mL·min^(-1),柱温为35℃,进样量为10μL。结果:酸性橙Ⅱ的浓度在0.000299~0.074790 mg·mL^(-1)范围内与其峰面积的线性关系良好(r=0.9999),平均加样回收率为100.1%(RSD=0.28%)。市售的31批红花中酸性橙Ⅱ的检出率为48%,检出量为6~329 mg·(100 g)^(-1)。结论:本法简便、快速、准确。可用于染色红花中酸性橙Ⅱ的测定。市售红花染色现象严重。
Objective:To establish an accurate method for the determination of Acid orange Ⅱ and abserve its contamination in Flos Carthami by HPLC. Method: HPLC was performed on DiamonsilTM C18 column(250 mm × 4. 6 mm,5 μm)at the 35 ℃ ,the mobile phase was consisted of 0. 025 mol· L^-1 potassium dihydrogen phosphate solution( content 0. 2% triethylamine, adjusted to pH 3.0 with Phosphoric acid ) - acetonitrile ( 55 : 45 ), the detection wavelength was 484nm,the flow rate was 1.0 mL ·min^-1 ,the temperature of column was 40 ℃ ,the sample was 10 μL. Results. The linear range of Acid orange 11 was 0. 000299 - 0. 074790 mg·mL^- 1 ( r = 0. 9999 ), and the average recovery was 100. 1% (RSD = 0.28 % ). The detective rate of 31 shares of Flos Carthami was 48 %, the concentration were 6 -329 mg·(100g)^-1. Conclusion :The method is simple, rapid and accurate. Acid orange Ⅱ is added to pigmentation of the Flos Carthami is populer and serious to human health.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第11期1794-1796,共3页
Chinese Journal of Pharmaceutical Analysis