色谱柱选择对六味安消胶囊中大黄素和大黄酚含量测定的影响

doi:10.3724/SP.J.1123.2016.08008

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

色谱柱选择对六味安消胶囊中大黄素和大黄酚含量测定的影响

王明娟, 刘雅丹, 胡晓茹, 何风艳, 项新华, 戴忠, 于健东, 马双成

中国食品药品检定研究院, 北京 100050

收稿日期:2016-08-07 出版日期:2016-11-08 发布日期:2016-11-03
通讯作者: 戴忠, 马双成
基金资助:
国家“十二五”专项（2014ZX09304307-002）.

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

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).

摘要/Abstract

摘要：

以中国药典收载的六味安消胶囊中大黄素与大黄酚的含量测定方法为典型案例，揭示了色谱柱是影响HPLC质量控制方法测定结果准确性的关键风险因素。参加能力验证的155家实验室均采用方法规定的C₁₈柱，但由于不同品牌C₁₈柱间的选择性差异，有20家实验室的分析结果中大黄素峰与样品水解产物的色谱峰共流出，导致测定结果明显偏离正常值。统计结果表明，A型（早期开发、硅羟基残留较多）和E型（内嵌极性基团或以极性基团封尾）C₁₈柱更适于六味安消胶囊中大黄素与大黄酚的含量测定，这可能是因为大黄素和大黄酚结构中含有多个酚羟基，能与A型柱的残留硅羟基或E型柱内嵌/封尾的极性基团相互作用，从而增强其保留行为有关。建议相关实验室在制订HPLC质量控制方法时应特别注重色谱柱的耐用性考察，并尝试采用国外色谱柱分类数据库科学地指导色谱柱的选择，尽量采用难分离物质对作为系统适用性指标，完善质量标准，减少由于色谱柱选择不适宜导致测定结果不准确的风险。

关键词: 大黄酚, 大黄素, 高效液相色谱, 关键风险因素, 六味安消胶囊, 色谱柱选择

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

中图分类号:

O658

王明娟, 刘雅丹, 胡晓茹, 何风艳, 项新华, 戴忠, 于健东, 马双成. 色谱柱选择对六味安消胶囊中大黄素和大黄酚含量测定的影响[J]. 色谱, 2016, 34(11): 1077-1083.

WANG Mingjuan, LIU Yadan, HU Xiaoru, HE Fengyan, XIANG Xinhua, DAI Zhong, YU Jiandong, MA Shuangcheng. Influence of column selection in assay of emodin and chrysophanol in Liuwei Anxiao capsules[J]. Chinese Journal of Chromatography, 2016, 34(11): 1077-1083.

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色谱柱选择对六味安消胶囊中大黄素和大黄酚含量测定的影响

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

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