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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。
The method of determination of emodin and chrysophanol in Liuwei Anxiao Capsule which is contained in Chinese Pharmacopoeia is a typical case and reveals that the chromatographic column is a key risk factor affecting the accuracy of the determination result of HPLC quality control method. The 155 laboratories that participated in proficiency testing adopted the C18 column method, but because of the selectivity difference between C18 columns of different brands, chromatographic peaks of emodin peak and sample hydrolyzate were co-eluted in the analysis results of 20 laboratories, Resulting in the measurement results deviate significantly from normal. The statistical results show that the C18 column of type A (early development with more silanol residues) and type E (with or without polar groups) is more suitable for the combination of emodin and chrysophanol This may be due to the fact that the structures of emodin and chrysophanol contain multiple phenolic hydroxyl groups that can interact with the residual silanol groups of the A-type column or the polar groups of the E-type column in / Retention behavior related. It is suggested that relevant laboratories should pay special attention to the durability investigation of HPLC when formulating HPLC quality control methods and try to guide the selection of chromatography column scientifically using foreign classification database to make use of difficult to separate substances as the index of system suitability Quality standards to reduce the risk of inaccurate assay results due to inappropriate column selection.