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HPLC-DAD波长切换法同时测定枳黄通泻颗粒中13种成分

Simultaneous determination of 13 components of Zhihuang Tongxie Granules by HPLC-DAD wavelength switching method

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【作者】 林义平田斌瞿孝兰宋英YUAN Qiang-hua

【Author】 LIN Yi-ping;TIAN Bin;QU Xiao-lan;YUAN Qiang-hua;SONG Ying;Chengdu University of Traditional Chinese Medicine;The Affiliated Hospital of Chengdu University of Traditional Chinese Medicine;

【通讯作者】 宋英;

【机构】 成都中医药大学成都中医药大学附属医院

【摘要】 目的:建立测定枳黄通泻颗粒中13种有效成分(辛弗林、紫丁香苷、木兰花碱、柚皮苷、橙皮苷、新橙皮苷、芦荟大黄素、大黄酸、大黄素、和厚朴酚、厚朴酚、大黄酚、大黄素甲醚)的方法,为枳黄通泻颗粒含量测定及质量控制提供参考。方法:采用Agilent Zorbax SB-C18 (250 mm×4.6 mm,5 μm)色谱柱;乙腈(A)-0.1%磷酸水(B)为流动相;梯度洗脱;流速1.0 mL·min-1;检测波长:0~10 min:275 nm (辛弗林);10~35 min:260 nm (紫丁香苷、木兰花碱);35~60 min:280 nm (柚皮苷、橙皮苷、新橙皮苷);60~96 min:254 nm (芦荟大黄素、大黄酸、大黄素);96~104 min:294 nm (厚朴酚、和厚朴酚);104~120 nm:254 mn (大黄酚、大黄素甲醚)。结果:本方法下各成分分离度良好,阴性无干扰,专属性强;辛弗林、紫丁香苷、木兰花碱、柚皮苷、橙皮苷、新橙皮苷、芦荟大黄素、大黄酸、大黄素、和厚朴酚、厚朴酚、大黄酚、大黄素甲醚分别在20.03~200.31μg·mL-1(r=0.999 6)、5.12~51.20 μg·mL-1 (r=0.9999)、11.10~110.98 μg·mL-1 (r=0.999 8)、24.89~248.92 μg·mL-1 (r=0.999 9)、10.11~101.14 μg·mL-1 (r=0.999 9)、23.44~234.39μg·mL-1 (r=0.999 9)、5.23~52.31μg·mL-1 (r=0.999 8)、1.91~19.15 μg·mL-1 (r=0.999 8)、4.05~40.48 μg·mL-1(r=0.999 8)、12.52~125.22 μg·mL-1 (r=0.999 6)、43.43~434.34 μg·mL-1(r=0.999 7)、10.46~104.60 μg·mL-1(r)=0.999 7、2.39~23.91 μg·mL-1(r=0.999 7)浓度范围内线性关系良好;精密度、稳定性、重复性的RSD小于3.00%;加样回收率在95.17%~104.59%之间,RSD小于3.00%。结论:该方法准确可靠、重复性好,可用于枳黄通泻颗粒的含量测定及质量控制。

【Abstract】 Objective:To establish a method for the determination of 13 active components of Zhihuang Tongxie Granules(synephrine,syringin,magnoflorine,naringin,hesperidin,neohesperidin,aloe-emodin,rhein,emodin,honokiol,magnolol,chrysophanol,and physcion),and to provide reference for the content determination and quality control of Zhihuang Tongxie Granules.Method:The analysis was performed on Agilent Zorbax SB-C18 column(250 mm×4.6 mm,5 μm) with mobile phase consisting of acetonitrile-0.1% phosphoric acid for gradient elution at a flow rate of 1.0 mL·min-1.The detection wavelengths were 275 nm(0~10 min) for synephrine,260 nm(10~35 min) for syringing and magnoflorine,280 nm(35~60 min) for naringin,hesperidin and neohesperidin,254 nm(60~90 min) for aloe-emodin,rhein,and emodin,294 nm(90~104 min) for magnolol,and honokiol,254 nm(104~120 min) for chrysophanol,and physcion,respectively.Result:The separation degree of each component was good,negative without interference with strong specificity.The linear relationship was good within the concentration range of synephrine,syringin,magnoflorine,naringin,hesperidin,neohesperidin,aloe-emodin,rhein,emodin,honokiol,magnolol,chrysophanol,and physcion,which were 20.03~200.31μg·mL-1(r=0.9996),5.12~51.20 μg·mL-1(r=0.9999),11.10~110.98μg·mL-1(r=0.9998),24.89~248.92μg·mL-1(r=0.9999),10.11~101.14μg·mL-1(r=0.9999),23.44~234.39μg··mL-1;(r=0.9999),5.23~52.31 μg·mL-1(r=0.9998),1.91~19.15 μg·mL-1(r=0.9998),4.05~40.48 μg·mL-1(r=0.9998),12.52-125.22μg·mL-1(r=0.9996),43.43~434.34μg·mL-1(r=0.9997),10.46~104.60 μg·mL-1(r=0.9997),2.39~23.91μg··mL-1(r=0.999 7).RSD of precision,stability and repeatability was less than 3.00%.The recovery was between 95.17% and 104.59%,with RSD less than3.00%.Conclusion:The method is accurate,reliable and repeatable,and can be used for the content determination and quality control of Zhihuang Tongxie Granules.

  • 【文献出处】 中药与临床 ,Pharmacy and Clinics of Chinese Materia Medica , 编辑部邮箱 ,2021年03期
  • 【分类号】R286.0
  • 【被引频次】2
  • 【下载频次】72
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