以化妆品中23种防腐剂检测方法为例,探讨色谱柱选择对液相色谱方法测定结果的影响。参照《化妆品安全技术规范》甲基异噻唑啉酮等23个组分的检验方法,在2台不同的高效液相色谱仪上用15款不同品牌、型号的C_(18)色谱柱检测23种防腐剂,计...以化妆品中23种防腐剂检测方法为例,探讨色谱柱选择对液相色谱方法测定结果的影响。参照《化妆品安全技术规范》甲基异噻唑啉酮等23个组分的检验方法,在2台不同的高效液相色谱仪上用15款不同品牌、型号的C_(18)色谱柱检测23种防腐剂,计算色谱峰的理论塔板数和分离度,对23种组分的分离效果进行分析,并应用USP(United States Pharmacopeia)数据库和PQRI(Product Quality Research Institute)数据库等2种等效色谱柱选择方法,对不同色谱柱的分离效果及等效性进行评价和预测。实验结果表明,15款色谱柱对23种防腐剂的分离效果差异显著,仅有2款色谱柱可以实现23种组分的完全分离。USP和PQRI数据库中2种等效色谱柱选择方法均无法预测出合适的等效色谱柱,对23种防腐剂的液相色谱分析参考价值均较小。色谱柱是影响23种防腐剂液相色谱法测定结果准确性的关键因素,有关实验室在应用该方法时,应考虑色谱柱选择性差异。化妆品基质复杂,如何在现有研究成果的基础上,开发色谱柱的筛选和预测评价体系,进而指导实际样品的分离是下一步研究的重点、难点。建议有关部门在制修订检测方法时,注重色谱柱的耐用性考察,完善系统适应性指标,细化色谱柱分类和增加描述信息,指导色谱柱的合理选择,从而规避由于色谱柱使用过程中选择依据缺失而导致测定结果不准确的风险。展开更多
Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it ...Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it is a challenge to obtain a baseline separation of ASPM components.Meanwhile,in some cases it was found that the results obtained by different brands of C_（18） columns were significantly different,indicating the necessity of a rational column selection for the separation of ASPM components.In this paper,we attempted to facilitate column selection for the analysis of ASPM using the database of the column characterization system established by Leuven University.With the CAPCELL PAK MG C_（18）（250 mm×4.6 mm,5μm） as the reference column,three groups of columns（F2 group：similar selectivity;2F6：intermediate ranked group;F6 group： different selectivity,compared to the reference column） were selected,and their performances in the separation of ASPM components were evaluated under the chromatographic conditions described in Chinese Pharmacopoeia monograph.A good relationship was demonstrated between the ranking of columns and their selectivity in the separation of ASPM components,indicating the column classification system established by Leuven University was a helpful tool in the selection of suitable columns for the analysis of ASPM,a complex mixture of basic compounds.展开更多
文摘以化妆品中23种防腐剂检测方法为例,探讨色谱柱选择对液相色谱方法测定结果的影响。参照《化妆品安全技术规范》甲基异噻唑啉酮等23个组分的检验方法,在2台不同的高效液相色谱仪上用15款不同品牌、型号的C_(18)色谱柱检测23种防腐剂,计算色谱峰的理论塔板数和分离度,对23种组分的分离效果进行分析,并应用USP(United States Pharmacopeia)数据库和PQRI(Product Quality Research Institute)数据库等2种等效色谱柱选择方法,对不同色谱柱的分离效果及等效性进行评价和预测。实验结果表明,15款色谱柱对23种防腐剂的分离效果差异显著,仅有2款色谱柱可以实现23种组分的完全分离。USP和PQRI数据库中2种等效色谱柱选择方法均无法预测出合适的等效色谱柱,对23种防腐剂的液相色谱分析参考价值均较小。色谱柱是影响23种防腐剂液相色谱法测定结果准确性的关键因素,有关实验室在应用该方法时,应考虑色谱柱选择性差异。化妆品基质复杂,如何在现有研究成果的基础上,开发色谱柱的筛选和预测评价体系,进而指导实际样品的分离是下一步研究的重点、难点。建议有关部门在制修订检测方法时,注重色谱柱的耐用性考察,完善系统适应性指标,细化色谱柱分类和增加描述信息,指导色谱柱的合理选择,从而规避由于色谱柱使用过程中选择依据缺失而导致测定结果不准确的风险。
文摘Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of spiramycin.In addition to the four main components,more than seventy minor components could be present in ASPM.Thus,it is a challenge to obtain a baseline separation of ASPM components.Meanwhile,in some cases it was found that the results obtained by different brands of C_（18） columns were significantly different,indicating the necessity of a rational column selection for the separation of ASPM components.In this paper,we attempted to facilitate column selection for the analysis of ASPM using the database of the column characterization system established by Leuven University.With the CAPCELL PAK MG C_（18）（250 mm×4.6 mm,5μm） as the reference column,three groups of columns（F2 group：similar selectivity;2F6：intermediate ranked group;F6 group： different selectivity,compared to the reference column） were selected,and their performances in the separation of ASPM components were evaluated under the chromatographic conditions described in Chinese Pharmacopoeia monograph.A good relationship was demonstrated between the ranking of columns and their selectivity in the separation of ASPM components,indicating the column classification system established by Leuven University was a helpful tool in the selection of suitable columns for the analysis of ASPM,a complex mixture of basic compounds.
