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[摘要]
目的 基于一法多用策略,建立了在线二维多中心切割液相色谱同时测定三七、人参及其相关产品中人参皂苷Rg1、Re、Rf、Rb1、Rb2、Rb3、Rc、Rd的方法。方法 按照产品的不同类别和制备工艺,分别采用相应的样品制备方法,对于原药材及其复方中药固体制剂,采用加压溶剂萃取法,分别采用三氯甲烷和水饱和正丁醇的2步溶剂提取;优化了一维和二维色谱分离条件,包括色谱柱选择、梯度洗脱等,分别采用Phenyl-x和C18柱作为一维和二维色谱柱,根据各目标物在一维色谱柱上的出峰时间,设置切割时间窗口,将各组分分别转移至6个定量环中,交替储存目标物馏分。第二维分离采用2.6 μm颗粒的核-壳柱实现了8次的快速循环分离,完成8个目标物的测定。结果 8种目标待测物在药材、提取物和中药复方等基质均可获得较好的分离和定量,线性相关系数r>0.999,连续进样的精密度RSD在0.52%~1.53%,方法回收率在94.57%~103.47%,检出限在0.041~0.18 μg/mL。结论 本方法可准确对不同样品基质中的8种人参皂苷进行定量测定,结合8种人参皂苷的相对比例变化,可对人参、三七及其相关产品进行质量评价。
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[Abstract]
Objective To establish a rapid method for the simultaneous quantification of eight ginsenosides in Notoginseng Radix et Rhizoma (NRR), Ginseng Radix et Rhizoma (GRR), and their related products by multi hearting-cutting two dimensional liquid chromatography based a "monomethod-heterotrait matrix" (MHM) strategy. Methods Corresponding sample preparations were applied to samples, which were different in either product forms or preparation processes. Pressured liquid extraction (PLE) was developed for the raw herbs and related solid-state Chinese patent medicine using two-steps solvent extraction with chloroform and water-saturated n-butanol. One and two dimensional separation conditions including columns selection and gradient elution were optimized systematically. Phenyl-X and C18 were confirmed as 1D and 2D columns, respectively. Eight targeting ingredients were cut alternately into six loops by starting-to-ending time of peaks in 1D column. 2D rapid separation for eight cycles was achieved on core-shell column with 2.6 μm particle to complete eight compounds quantitation. Results The eight targeting analytes were well separated and quantified in 50 min in different sample matrix (raw herbs, extract, and Chinese patent medicine). Method validation was performed in terms of linearity (r≥0.999), precision (0.52%-1.53%), and recovery (ranged from 94.57% to 103.47%), and the LODs (S/N=3:1) of the eight analytes varied from 0.041 to 0.18 μg/mL respectively. Conclusion Eight ginsenosides could be quantified accurately for different sample matrix. Combined with its relative proportions of eight ginsenosides, quality evaluation for NRR, GRR, and their related products could be performed scientifically.
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