Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (11): 1077-1083.DOI: 10.3724/SP.J.1123.2016.08008

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Influence of column selection in assay of emodin and chrysophanol in Liuwei Anxiao capsules

WANG Mingjuan, LIU Yadan, HU Xiaoru, HE Fengyan, XIANG Xinhua, DAI Zhong, YU Jiandong, MA Shuangcheng   

  1. National Institutes for Food and Drug Control, Beijing 100050, China
  • Received:2016-08-07 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    National "12th Five-Year" Projects (No. 2014ZX09304307-002).

Abstract:

Column selection is a factor of critical risk that may influence the accuracy of high performance liquid chromatography (HPLC) method. Assay of emodin and chrysophanol in Liuwei Anxiao capsules described in Chinese Pharmacopeia was taken as a typical example. Though 155 laboratories in the proficiency testing program all used C18 columns, the 20 ones obtained incorrect results due to the co-elution of emodin and acid hydrolysis product of Liuwei Anxiao capsules in the selected C18 columns. Statistical results showed that A-type (early developed columns with higher silicon hydroxyls residues) and E-type (with embedded or end-capping polar group) C18 columns were more suitable for the assay of emodin and chrysophanol in Liuwei Anxiao capsules. It might attribute to the presence of phenolic hydroxyl groups in emodin and chrysophanol and interact with residual silicon hydroxyls in A-type columns or polar groups in E-type ones. To reduce the risk of unsuitable column selection, related laboratories should pay more attention to the robustness of columns when HPLC methods are established. The column selection for robustness could be based on peer-reviewed column classification databases, and the resolution of critical pair should be recommended to use as system suitability parameter.

Key words: chrysophanol, column selection, critical risk factor, emodin, high performance liquid chromatography (HPLC), Liuwei Anxiao capsules

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